As the paragraph descriping shows that 33454-82-9 is playing an increasingly important role.
With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.33454-82-9,Lithium trifluoromethanesulfonate,as a common compound, the synthetic route is as follows.
Preparation 4: Ethyl Z-5-methyl-3-(trifluoromethylsulfonyloxy)-2-hexenoateA 20L jacketed reactor was charged with DCM (2.45L), ethyl 3-oxo-5- methylhexanoate (163.3g; 1 eq) and lithiunn triflate (295.86g; 2eq) under an inert atmosphere. The resulting white suspension was stirred and cooled to 0C. N, N- Diisopropylethylamine (134.8g; 182ml; 1 .1 eq) was added over 10 minutes at <10C. The suspension was stirred for 20 minutes at 0C, then triflic anhydride (294.28g; 175ml; 1 .1 eq) was added slowly to the mixture over 30 minutes at <10C. The suspension was stirred at 0C for 1 hour.A sample of the reaction mixture was taken and partitioned between MTBE and sat. NH4CI (1 ml each). The aqueous layer was extracted with MTBE (1 ml) and the combined organic extracts were filtered through cotton wool/MgSO . Analysis by GC indicated that less than 2% starting material remained.The mixture was allowed to warm from 0 to 25C over 1 hr whilst quenching with sat. NH4CI (980ml). DCM (490ml) was added and the mixture was stirred for 5 minutes, then allowed to settle and the layers were separated. The aqueous layer was extracted with DCM (490ml). The combined organic phases were then washed with 1 M HCI (2 490ml), water (490ml) and 20% brine (490ml), then stirred for 30 minutes with MgSO4 (~165g) for 15-30 minutes. The solids were removed by filtration and washed with DCM (165ml). The filtrate was concentrated under vacuum at <40C to give an orange/brown oil containing crystalline solids. The crude product was triturated with MTBE (980ml). The mixture was filtered and the solids were washed with MTBE (2 x 165ml). The filtrate was concentrated under vacuum at <40C to give the title product as an orange/brown oil: overall yield 271 g (94%; corrected for 2.1 %w/w MTBE content); 87.7% area purity by GC. 1 H NMR (CDCI3, delta= 7.20): delta 0.94 (6H, d, J = 6.7 Hz), 1 .24 (3H, t, J = 7.2 Hz), 1 .89 (1 H, hept, J = 6.8 Hz), 2.17 (2H, d, J = 7.2 Hz), 4.18 (2H, q, J = 7.2 Hz), 5.67 (1 H, s) ppm., 33454-82-9
As the paragraph descriping shows that 33454-82-9 is playing an increasingly important role.
Reference£º
Patent; PFIZER MANUFACTURING IRELAND; BURRELL, Adam James Musgrave; MARTINEZ, Carlos Alberto; MCDAID, Paul Oliver; O’NEILL, Padraig Mary; WONG, John Wing; WO2012/25861; (2012); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI