反应详情

温度

1 °C

In a three necked flask, under argon, a solution 4-hydroxymethyl-1-(4-methoxy-benzyl)-pyrrolidin-2-one a2 (4.3 g, 0.018 mol) and Et3N (8.9 ml) in CH2Cl2 (25 ml) cooled down to −10° C. Pyridine-SO3 (10.1 g, 0.064 mol, 3.5 eq) is added by portions and the temperature raised up to 1° C. After 3 h at −10° C., the reaction is quenched with water (100 ml) and extracted with CH2Cl2 (3 times). The organic phase is washed with successively a 1M solution of KHSO4, water, brine, dried over MgSO4, filtered and evaporated in vacuo to give the crude aldehyde a3 (3.2 g, 87%). It is dried several times by azeotropic distillation with toluene and used as such in the next step.

1. customthe reaction is quenched with water (100 ml)
2. extractionextracted with CH2Cl2 (3 times)
3. washThe organic phase is washed with successively a 1M solution of KHSO4, water, brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated in vacuo