HRID1710447

反应详情

EQUATION

反应方程式

HRID 1710447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 60% NaH in mineral oil (115 mg, 2.9 mmol) and 1H-indole-2,6-dicarboxylic acid diethyl ester (500 mg, 1.9 mmol) in DMF (3 mL) was stirred at room temperature for 0.5 h. Then bromo-acetonitrile in DMF (1 mL) was added and the reaction was warmed to 77° C. and kept at this temperature overnight. The reaction was cooled and quenched with ice water. A large amount of precipitate formed which was filtered and rinsed with water, followed by cold ether. The wet cake was dried in the vacuum oven (50° C.) to give 585 mg of 1-cyanomethyl-1H-indole-2,6-dicarboxylic acid diethyl ester.

WORKUP

后处理

  1. temperaturethe reaction was warmed to 77° C.
  2. customkept at this temperature overnight
  3. temperatureThe reaction was cooled
  4. customquenched with ice water
  5. customA large amount of precipitate formed which
  6. filtrationwas filtered
  7. washrinsed with water
  8. customThe wet cake was dried in the vacuum oven (50° C.)