HRID2226934

反应详情

EQUATION

反应方程式

HRID 2226934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 10% Pd/C (1.2 g) in 50 ml of ethanol was added a solution of 1,2,3,4-tetrahydro-7-phenylmethoxy-4-methylcyclopent[b]indole-2-methanol (8.4 g, 0.027 mole) in 200 ml of ethanol in a Parr hydrogenation bottle. After shaking at 50° C., under 50 psi hydrogen for two hours, the mixture was cooled, filtered, and then concentrated to a dark oil. The oil was eluted on a silica gel column with ethyl acetate/dichloromethane (1:2) via HPLC. The desired fractions were combined and then concentrated to a light yellow solid. The material was triturated with ether and dried to give 4.0 g (66%) of the product as an off-white solid, m.p. 153°-4° C.

WORKUP

后处理

  1. temperaturethe mixture was cooled
  2. filtrationfiltered
  3. concentrationconcentrated to a dark oil
  4. washThe oil was eluted on a silica gel column with ethyl acetate/dichloromethane (1:2) via HPLC
  5. concentrationconcentrated to a light yellow solid
  6. customThe material was triturated with ether
  7. customdried