HRID1587865

反应详情

EQUATION

反应方程式

HRID 1587865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureOn cooling to room temperature the mixture
  2. concentrationwas concentrated in vacuo
  3. additionWater (20 ml) was added to the residue
  4. extractionthe mixture was extracted with dichloromethane (3×20 ml)
  5. dry with materialThe combined dichloromethane extracts were dried (Na2SO4)
  6. concentrationconcentrated in vacuo
  7. customto give a gum which
  8. customwas purified by column chromatography on silica eluting with dichloromethane
  9. additioncontaining methanol (0% up to 10%)
  10. concentrationconcentrated in vacuo