HRID2226931

反应详情

EQUATION

反应方程式

HRID 2226931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 1,2,3,4-tetrahydro-7-phenylmethoxy-4-methycyclopent[b]indole-2-carboxylic acid ethyl ester (2.0 g, 0.006 mole) in 50 ml of dry tetrahydrofuran, was added lithium aluminum hydride (1M solution in tetrahydrofuran, 10 ml, 0.01 mole). After stirring at 70° C. for one hour, the mixture was cooled, quenched with 2 ml of saturated ammonium chloride solution, filtered, and the filtrate concentrated to a brown oil, ~2 g. This oil was eluted on a silica gel column with 10% methanol/dichloromethane via HPLC. The desired fractions were combined and concentrated to a tan oil, which solidified on standing to give 1.3 g of the product, m.p. 83°-85° C.

WORKUP

后处理

  1. temperaturethe mixture was cooled
  2. customquenched with 2 ml of saturated ammonium chloride solution
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated to a brown oil, ~2 g
  5. washThis oil was eluted on a silica gel column with 10% methanol/dichloromethane via HPLC
  6. concentrationconcentrated to a tan oil, which