反应详情

Potassium cyanide (13.0 g, 0.2M) was stirred in absolute ethanol and ethyl cyanoacetate (22.6 g, 0.2M) and paraformaldehyde (6.0 g, 0.2m) were added at ambient temperature. After 5 minutes the white suspension was heated under reflux conditions for 12 minutes, and the orange solution was evaporated to dryness in vacuo at below 25° C. to give a buff solid. The solid (the potassium salt) was dissolved in water (400 ml), acidified to pH 5 with 2M hydrochloric acid solution, giving a red oil. This mixture was extracted with dichloromethane and the extracts dried and evaporated to dryness in vacuo to give the title compound as a red oil (23.5 g), 1H NMR (CDCl3) d 4.3 (2H, q), 3.95 (1H, t), 3.0 (2H, d), 1.35 (3H, t); identical with an authentic sample. Distilled material had b.p. 132-136° C. at 0.5mmHg. Yield : 77%.

1. temperatureAfter 5 minutes the white suspension was heated under reflux conditions for 12 minutes
2. customthe orange solution was evaporated to dryness in vacuo at below 25° C.
3. customto give a buff solid
4. customgiving a red oil
5. extractionThis mixture was extracted with dichloromethane
6. customthe extracts dried
7. customevaporated to dryness in vacuo