Day: August 21, 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.554-95-0,Benzene-1,3,5-tricarboxylic acid,as a common compound, the synthetic route is as follows.

20.00 g of trimesic acid was dissolved in 350 mL of methanol, 5 mL of 18 mol / L concentrated sulfuric acid catalyst was added slowly and refluxed at 73 oC for 24 h.The solvent was evaporated under reduced pressure, 60 mL of chloroform was added until just dissolved, and 130 mL of a 100 g / L saturated sodium bicarbonate solution was added until the pH was neutral.The organic phase was separated and the solvent was evaporated under reduced pressure and dried under vacuum at 80 C to give 23.03 gTrimellitic acid methyl ester(96% yield).

The synthetic route of 554-95-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Jilin Chemical College; Gao Wenxiu; Wang Jisi; Lou Dawei; Yu Dandan; Zhang Zhihui; Zhang Hao; (9 pag.)CN107501043; (2017); A;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

485-71-2, Cinchonidine is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Previous resolution of CPTA has been reported in U. S. Patent No. 3,517, 050, in which cinchonidine was used as the chiral base, and the (+)-enantiomer of CPTA precipitated as the diastereomeric salt. One major drawback to this procedure was that the desired (-)- enantiomer remained in the mother liquor, making separation of a pure (-)-enantiomer fraction difficult. [0092] This example shows the results of resolving a racemic mixture of CPTA using A variety of different chiral bases to obtain a solid enantiomerically enriched (-) -isomer. Unlike the previous method, methods of the present invention allow the solid enantiomerically enriched (-) -CPTA to be readily isolated from the solution. [0093] Racemic CPTA was prepared by the potassium hydroxide hydrolysis of racemic halofenate. For chiral base screening, equal molar mixtures of CPTA and the chiral base were mixed in ethanol, methanol and acetone in glass vials, and the solutions were allowed to stand undisturbed. After holding overnight at ambient temperature, the samples that remained in solution were placed in a refrigerator at 5 C. After holding overnight in the refrigerator, a small amount of water was added to the samples that remained a solution in ethanol. After four days at ambient temperature, the aqueous ethanol solutions were placed back in the refrigerator. All of the samples remained in the refrigerator, and were periodically checked for precipitate formation over the course of a month. A list of the bases and solvent conditions examined, and temperatures at which crystalline salts were found is shown in Table 1. Table 1. Bases Examined for CPTA Resolution. Solvent System Base EtOH EtOH (aq) Acetone MeOH S- (-)-Methylbenzylamine E E E E Quinine C (22 C) C (22 C) C (22 C) Quinidine E E L-Tyrosine Hydrazide C (22 C) L-Leucine Methyl Ester Hydrochloride* E E 1-2-Amino-l-butanol E E E E Brucine E E E E (S)-(+)-2-Pyrrolidine-methanol E E E E (S)-(+)-2-Amino-3-methyl-1-butanol E (S)- (+)-2-Amino-1-propanol E (S)-(-)-2-Amino-3-phenyl-1-propanol E (1 S, 2S)-(+)-Pseudoephedrine E E E E (1S,2S)-(+)-2-Amino-1-phenyl-1,3-propanediol E E E E (1 S, 2S)-(+)-2-Amino-1-(4-nitrophenyl)-1, 3-propandiol C (5 C) (lR, 2S)- (-)-Norephedrine E E E E (1R,2R)-(-)-Ephedrine (1R,2R)-(-)-2-Amino-1-(4-nitrophenyl)-1, 3-propandiol C (22 C) (+)-Cinchonone E E E E (-)-Cinchonidine C (22 C) (-)-Strychnine E E E E E-Evaluated C-Crystallized at (Temperature) *-With 1 MOL/MOL of Aqueous Sodium Hydroxide [0094] Four chiral bases, quinine, L-tyrosine hydrazide, (-) -cinchonidine, and both enantiomers of 2-amino-1-(4-nitrophenyl)-1, 3-propandiol, were found to give crystalline salts from racemic CPTA. For samples that crystallized, the solid was isolated by filtration, and both the solid phase and mother liquor were analyzed by chiral HPLC to determine the enantiomeric composition of both streams. The results from the screen are shown in Table 2. Three of the bases shown in Table 2 gave the (+) -enantiomer enrichment in the solid phase. Table 2. Results from Chiral Base Screen. Solid Mother Liquor % Yield Base % (+) % (-) % (+) % (-) Calculated Solvent Temp C L-Tyrosine Hydrazide Acetone 22 86. 6 13. 4 40. 7 59.3 20.3 (-) -Cinchonidine Ethanol 22 66.8 33.2 12. 0 88.0 69.3 (1S, 2S)- (+)-2-Amino-1- (4- Ethanol 22 93. 2 6.8 28.5 71. 5 33. 2 nitrophenyl)-1, 3-propandiol Quinine Ethanol 22 39.9 60.1 60.1 39.9 50.1 Acetone 22 28. 2 71.8 58.9 41. 1 28. 9 Acetone* 5 23. 0 77.0 83. 5 16. 5 55. 4 Methanol 22 25. 8 74.2 53.0 47. 0 10. 9 2-Propanol 30 43. 2 56.8 64.3 35. 7 67. 6 2-Propanol** 30 40. 4 59.6 78.8 21. 1 75. 0 2-Propanol* 21 42.3 57.7 59.1 40.9 53.9 *-More Dilute **-Slower Cooling Profile [0095] Included in Table 2 is the percent yield of solid calculated from the isomeric ratio in the solid and mother liquor streams. The equation used is shown below. The maximum theoretical yield with 100% isomeric purity is 50%. Yields over 50% indicate inclusion of the other isomer. Equation to calculate yield from isomer ratios. Set: a = area % Component 1 in starting material; b = area % Component 2 in starting material; x = area % Component 1 in isolated; y = area % Component 2 in isolated; w = area % Component 1 in mother liquor; z = area % Component 2 in mother liquor; E = g material isolated; F = g material in mother liquor. And: A+B=100% ; E+F=L Then: XE+WF=A ; YE+ZF=B Solving: XE + W (1-E) = A ; YE + Z (1-E) = B E = isolated yield = (A-W)/ (X-W) = (B-Z)/ (Y-Z)This example shows representative results of chiral resolution screening in ethanol using a variety of chiral bases. [0113] A sample of 1.16 g (3.51 mmol) of CPTA was dissolved in 6.98 g of ethanol to give a solution (0.431 mmol/g). Glass vials were individually charged with the amounts of each base listed in Table 5, and the amount of the ethanolic CPTA solution calculated to give a 1 to 1 molar ratio of acid to base was added. In some cases, a small amount of ethanol was added to wet the base prior to addition of the CPTA solut…

As the paragraph descriping shows that 485-71-2 is playing an increasingly important role.

Reference£º
Patent; METABOLEX, INC.; WO2004/112774; (2004); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

119-91-5, 2,2′-Biquinoline is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Cu(NO3)2.4H2O (103 mg, 0.4 mmol) and Na(dca) (71 mg,0.8 mmol) were dissolved in ethanol (60 ml) and stirred withheating to 343 K. To this hot solution, a solution of biq (205 mg, 0.8 mmol) in acetonitrile (75 ml) was added and stirring was continued for about 40 min. The resulting redsolution was filtered into a beaker and left undisturbed in thedark at room temperature. After 10 d, dark-green tabular crystals were obtained. The crystals were collected by filtration,washed with acetonitrile and dried in air [yield: 93 mg,26%, based on Cu(NO3)2.4H2O]. Elemental analysis (%)calculated for C44H24Cu2N16: C 58.47, H 2.68, N 24.79; found:C 58.36, H 2.71, N 24.86. IR (KBr, cm-1): 3631 (w), 3126 (w),3058 (w), 2347 (s), 2268 (s), 2210 (s), 2160 (s), 1618 (w), 1594(m), 1550 (w), 1509 (w), 1432 (w), 1381 (s), 1340 (m), 1290 (w),1214 (w), 1159 (w), 1102 (w), 971 (w), 914 (w), 819 (s), 781 (m),755 (m), 742 (m), 619 (w), 531 (w).

As the paragraph descriping shows that 119-91-5 is playing an increasingly important role.

Reference£º
Article; Poto??ak, Ivan; Bukrynov, Oleksandr; Raczova, KatarAna; ?i?mar, Erik; Vitushkina, Svitlana; Vahovska, Lucia; Du?ek, Michal; ?tarha, Pavel; Acta Crystallographica Section C: Structural Chemistry; vol. 74; 11; (2018); p. 1469 – 1476;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.294-90-6,1,4,7,10-Tetraazacyclododecane,as a common compound, the synthetic route is as follows.

1,4,7,10-Tetraazacyclododecane (10 mmol) was dissolved in methanol (15 ml). To the system was added triethylamine (2 ml), and then slowly dropwise added at room temperature ethyl trifluoroacetate (50 mmol). Upon the completion of dropwise addition, the mixture was allowed to react at room temperature over night, concentrated and then column separated (eluant: ethyl acetate) to obtain 4.1 g of a white solid, yield 89%, MS[M]+=460.3 m/e.

294-90-6 1,4,7,10-Tetraazacyclododecane 64963, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Patent; Beijing Molecule Science and Technology Co., Ltd.; EP2163553; (2010); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1970-80-5,(2,2-Bipyridine)-5-carboxylic acid,as a common compound, the synthetic route is as follows.

Compound 7 (600 mg, 0.56 mmol) was suspended in methylene chloride (15 ml), and compound 11 (0.5 g, 2.5 mmol),Triethylamine (0.6 ml, 4.33 mmol), DMAP (0.1 ml) was added. The solution was cooled with ice,WSC (1.7 g, 8.9 mmol) was added and the mixture was stirred for 24 hours. The solvent was concentrated to dryness and the crude product was purified by silica gel column chromatography to obtain 0.5 g (yield 36%) of TPE-Bipy.

As the paragraph descriping shows that 1970-80-5 is playing an increasingly important role.

Reference£º
Patent; DOJINDO LABORATORIES; SHINKAI, SEIJI; SHIGA, MASANOBU; OSETO, FUMIO; NOGUCHI, TAKAO; (18 pag.)JP6081152; (2017); B2;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.147-85-3,H-Pro-OH,as a common compound, the synthetic route is as follows.

Equimolar amounts of mandelic acid, or (R)-(-)-mandelic acid or (S)-(+)-mandelic acid or L-proline and potassium hydroxide (scale 0.1 mol) were dissolved in distilled water (100 mL). After clarity of solution equimolar amount of quaternary ammonium chloride in distilled water (80 mL) was added. The mixture was heated at 60 C for 5 h. The water was removed under reduced pressure (70 C, 30¡Á102 Pa). Anhydrous methanol was added and the mixture was allowed to stand overnight at room temperature. The crystalline potassium chloride was removed by filtration and methanol by distillation. The obtained residue was dried overnight in vacuum at 80 C.

147-85-3 H-Pro-OH 145742, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Article; Cybulski, Jacek; Wi?niewska, Anna; Kulig-Adamiak, Anna; Da?browski, Zbigniew; Praczyk, Tadeusz; Michalczyk, Alicja; Walkiewicz, Filip; Materna, Katarzyna; Pernak, Juliusz; Tetrahedron Letters; vol. 52; 12; (2011); p. 1325 – 1328;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

107-64-2, Dimethyldioctadecylammonium chloride is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

3. 576 g (3 mol) of 3,4-dichloronitrobenzene, 58 g (0.1 mol) of distearyldimethylammonium chloride and 139 g (2.4 mol) of potassium fluoride were reacted analogously to Example 1. After filtering with suction, the residue was dissolved in water, the organic phase was separated off and the combined organic phases were fractionated. 289 g (69%, relative to potassium fluoride employed) of 3-chloro-4-fluoronitrobenzene were obtained.

107-64-2 Dimethyldioctadecylammonium chloride 7879, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Patent; Hoechet AG; US5545768; (1996); A;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.122-18-9,N-Benzyl-N,N-dimethylhexadecan-1-aminium chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 4 N-(1H-pyrazol-1-ylmethyl)-N-(2,4-dimethyl-thien-3-yl)-chloroacetamide (process b) To a well stirred mixture of 19.35 g (0.095 mol) of N-(2,4-dimethyl-thien-3-yl)-chloroacetamide, 4.15 g (0.01 mol) of benzyldimethylhexadecyl-ammonium chloride, 40 g (1 mol) of sodium hydroxide, 200 ml of methylene chloride and 40 ml of water are added 17 g (0.11 mol) of solid 1-chloromethyl pyrazolehydrochloride at such a rate, that the temperature does not rise above 25. When the addition is completed, the reaction mixture is stirred an additional 21/2 hours at ambient temperature. Then 100 ml of water are added. The organic layer is separated, washed with three 200 ml portions of water, dried over Na2 SO4 and evaporated to dryness. The residue is chromatographed on a silica gel column. Elution with hexane-diethylether 1:1 affords the title compound as an analytically pure syrup which crystallized on chilling overnight at -20, m.p. 88-89 (recrystallized from diethyl ether).

As the paragraph descriping shows that 122-18-9 is playing an increasingly important role.

Reference£º
Patent; Sandoz Ltd.; US4666502; (1987); A;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.7173-51-5,N-Decyl-N,N-dimethyldecan-1-aminium chloride,as a common compound, the synthetic route is as follows.

Didecyldimethylammonium chloride (0.02 mol) was dissolved in distilled water and 0.015 mol of benzoic acid sodium salt was added. The solution was stirred at 80 C. for 7 h. The reaction mixture was extracted by chloroform. Chloroform phase was removed and washed with distilled, cold water until chloride ions were no longer detected using AgNO3. Then chloroform was removed. Obtainede benzoate in 85% yield was dried in vacuum. 1H NMR and 13C NMR (CDCl3) were obtained.

7173-51-5 N-Decyl-N,N-dimethyldecan-1-aminium chloride 23558, acatalyst-ligand compound, is more and more widely used in various.

Reference£º
Patent; Rogers, Robin D.; Daly, Daniel T.; Swatloski, Richard P.; Hough, Whitney L.; Davis, James Hilliard; Smiglak, Marcin; Pernak, Juliusz; Spear, Scott K.; US2007/93462; (2007); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI

56-54-2, (S)-(6-methoxyquinolin-4-yl)((1S,2R,4S,5R)-5-vinylquinuclidin-2-yl)methanol is a catalyst-ligand compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A solution of quinine/quinidine 5 in dry DMF (4 mL/mmol 5) was treated with dry NaH (2.8 equiv.) and the resulting mixture was stirred at r.t. for 2 h. Benzyl chloride or allyl bromide (1.1 equiv.) were added and the resulting mixture was stirred at r.t. for 20 h. After extraction with brine and EtOAc the organic phase was dried over Na2SO4, filtrated and evaporated to dryness, giving 9-O-allylated or 9-O-benzylated compounds 6 [26] in >87% yield and sufficient purity for the following steps.

The synthetic route of 56-54-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Schoergenhumer, Johannes; Otte, Stefan; Haider, Victoria; Novacek, Johanna; Waser, Mario; Tetrahedron; (2019);,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI