HRID1647790

反应详情

EQUATION

反应方程式

HRID 1647790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 95% LiAlH4 (2.20 g, 0.058 mol) in 60 mL of dry THF was added a solution of ethyl 5-nitro-3-indolepropionate (7.30 g, 0.028 g mol) in 100 mL of dry THF, at 0° C. under Ar. After stirring for 20 min the mixture was quenched by cautiously adding 3 mL of H2O. The resulting suspension was stirred for 10 min and then it was filtered and the filtercake was washed with additional THF. The filtrate was evaporated and the residue was taken up in ether, dried (Na2SO4) and evaporated, and the resulting solid was triturated with hexane to give the title compound (4.30 g, 70%) as a yellow solid, m.p. 107°-110° C.

WORKUP

后处理

  1. customat 0° C.
  2. customwas quenched
  3. additionby cautiously adding 3 mL of H2O
  4. stirringThe resulting suspension was stirred for 10 min
  5. filtrationit was filtered
  6. washthe filtercake was washed with additional THF
  7. customThe filtrate was evaporated
  8. dry with materialdried (Na2SO4)
  9. customevaporated
  10. customthe resulting solid was triturated with hexane