反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
A mixture containing 1-cyano-1,1-diphenyl-3-[N-{2-(2,3-dihydrobenzofur-5-yl)ethyl}-N-methylamino]propane (0.087 g), potassium hydroxide (0.074 g), ethanol (6 ml) and water (6 ml) was heated at 140° C. in a stainless steel pressure vessel for 48 hours. On cooling to room temperature the mixture was concentrated in vacuo. Water (20 ml) was added to the residue and the mixture was extracted with dichloromethane (3×20 ml). The combined dichloromethane extracts were dried (Na2SO4) and concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 10%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a glass, yield 0.056 g.
WORKUP
后处理
- temperatureOn cooling to room temperature the mixture
- concentrationwas concentrated in vacuo
- additionWater (20 ml) was added to the residue
- extractionthe mixture was extracted with dichloromethane (3×20 ml)
- dry with materialThe combined dichloromethane extracts were dried (Na2SO4)
- concentrationconcentrated in vacuo
- customto give a gum which
- customwas purified by column chromatography on silica eluting with dichloromethane
- additioncontaining methanol (0% up to 10%)
- concentrationconcentrated in vacuo