HRID1936710

反应详情

EQUATION

反应方程式

HRID 1936710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred suspension of 1-acetyl-7-(1-methylpiperidin-4-yl)-1,2,3,5-tetrahydropyrrolo[2,3-f]indole (D5, 0.55 g, 1.85 mmole) in ethanol (10 ml) and 10% sodium hydroxide solution (10 ml) was added sodium hydroxide pellets (0.50 g) and the resultant mixture was heated at reflux under argon for 18 hours. The mixture was cooled, diluted with water (75 ml) and extracted with dichloromethane (5×30 ml). The combined organic extracts were washed with brine, dried (MgSO4) and evaporated to dryness. The residue was triturated with diethyl ether and the solid filtered off and dried in vacuo to afford the title compound as an off-white powder (0.29 g).

WORKUP

后处理

  1. temperatureat reflux under argon for 18 hours
  2. temperatureThe mixture was cooled
  3. extractionextracted with dichloromethane (5×30 ml)
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated to dryness
  7. customThe residue was triturated with diethyl ether
  8. filtrationthe solid filtered off
  9. customdried in vacuo