HRID2307917

反应详情

EQUATION

反应方程式

HRID 2307917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 3-aminoindole-2-carboxylate [Prepared according to P. Unangst. J. Het. Chem., 1983, 20, 495] (5.0 g) in methanol (50 ml) was added sodium methoxide (6.5 g). The resulting mixture was stirred for 4 hours and then quenched with saturated ammonium chloride solution. The resulting mixture was extracted with dichloromethane, dried (MgSO4) and evaporated to give a gum which was purified by column chromatography using iso-hexane:ethyl acetate (1:4) as eluent to give the desired product (1.95 g, 42%); NMR d (CD3SOCD3), 3.8 (s, 3H), 5.7 (s, 2H), 6.8-6.9 (m, 1H), 7.2 (m, 2H), 7.7 (d, 1H); M/z (+) 191.1 (MH+).

WORKUP

后处理

  1. customquenched with saturated ammonium chloride solution
  2. extractionThe resulting mixture was extracted with dichloromethane
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customto give a gum which
  6. customwas purified by column chromatography