HRID490904

反应详情

EQUATION

反应方程式

HRID 490904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2M-Sodium hydroxide solution (0.75 ml, 1.5 mmol) was added to Intermediate 59 (0.248 g, 0.75 mmol) in ethanol (2 ml), and the mixture was heated at reflux for 16 hours. The reaction mixture was concentrated, diluted with water (1 ml) and acidified with 2M-hydrochloric acid (0.75 ml) to precipitate a solid which was collected by filtration to afford Intermediate 60 (0.168 g). LCMS showed MH+=305; TRET=1.86 min.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 16 hours
  3. concentrationThe reaction mixture was concentrated
  4. additiondiluted with water (1 ml)
  5. customto precipitate a solid which
  6. filtrationwas collected by filtration