반응 #2027415
ord-d019aebf564f4f3c958d6ed5753543a0
반응 방정식
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타A three-neck 5-mL flask fitted with a thermometer, mechanical stirrer, addition funnel, condenser and positive nitrogen atmosphere
- 2기타the flask was immersed in an ice bath
- 3온도to maintain a reaction temperature of 17°-19° C
- 4기타was then continued at ambient temperature
- 5기타(20° C.)
- 6기타for five hours
실험 절차
A three-neck 5-mL flask fitted with a thermometer, mechanical stirrer, addition funnel, condenser and positive nitrogen atmosphere was charged with EDC (200 mL), isobutyraldehyde (11.3 g, 0.157 mole), and 1,4-dichloro-2,3-butanediol (25.0 g, 0.157 mole). Concentrated sulfuric acid (23.2 g) was added dropwise to the agitated mixture over thirty minutes, during which time a slight exotherm was noticed and the flask was immersed in an ice bath to maintain a reaction temperature of 17°-19° C. Stirring was then continued at ambient temperature (20° C.) for five hours.