HRID508497

反应详情

EQUATION

反应方程式

HRID 508497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Barium hydroxide octahydrate (0.63 g, 2.0 mmol) was added to a solution of N-ethylcarbamate-5-methoxy-6-chloro-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole (61 mg, 0.2 mmol) in MeOH (4 mL), and stirred for 24 hours at reflux. The reaction mixture was cooled to room temperature and neutralized to pH=7 with aqueous HCl (50 mL, 1 M). The product was extracted with CH2Cl2, dried over MgSO4, and concentrated. The crude product was purified by reverse-phase liquid chromatography to afford the title compound. MS calculated for C13H16ClNO+H: 238, observed: 238.

WORKUP

后处理

  1. temperatureat reflux
  2. extractionThe product was extracted with CH2Cl2
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe crude product was purified by reverse-phase liquid chromatography