反应详情

Sodium methoxide (25% w/w in MeOH (44.62 g, 206.5 mmol)) was added slowly, (over 55 min.) whilst maintaining the temperature between 0 and 10° C., to ethyl 2-(dichloromethyl)-4,5-dihydro-1,3-thiazole-4-carboxylate (50.0 g, 206.5 mmol) in 50 mL of MeOH. An additional 50 mL of MeOH was added and stirred for 1 h. keeping the temperature below 10° C. DCM (125 mL) and water (71 mL) was added to the mixture and the organic layer was separated. The aqueous layer was extracted with a further 71 mL of DCM. The combined organic layers was dried over MgSO4 and evaporated in vacuo to give the crude product (34.6 g, 87%).

1. temperature(over 55 min.) whilst maintaining the temperature between 0 and 10° C.
2. customthe temperature below 10° C
3. customthe organic layer was separated
4. extractionThe aqueous layer was extracted with a further 71 mL of DCM
5. dry with materialThe combined organic layers was dried over MgSO4
6. customevaporated in vacuo