HRID363333

反应详情

EQUATION

反应方程式

HRID 363333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

The methanesulfonyl chloride (215 mg, 1.87 mmol) was added dropwise to a solution of the 3-(octahydroindolizin-7-yl)-5-amino-1H-indole (320 mg, 1.25 mmol) and triethylamine (0.5 ml) in 10 ml of dimethylformamide. The reaction was stirred at room temperature for 2.5 hours. The reaction was diluted with methanol and concentrated to give a dark semi-solid. This material was dissolved in a mixture of methylene chloride and water, made basic with an ammonium hydroxide solution, then extracted with methylene chloride. The extract was dried over sodium sulfate and concentrated to give a reddish brown oil. The material was purified on a flash column using silica gel (20% methanol in methylene chloride (ammonium hydroxide) as eluent) to give 210 mg of product. (49.7%).

WORKUP

后处理

  1. concentrationconcentrated
  2. customto give a dark semi-solid
  3. extractionextracted with methylene chloride
  4. dry with materialThe extract was dried over sodium sulfate
  5. concentrationconcentrated
  6. customto give a reddish brown oil
  7. customThe material was purified on a flash column