HRID21584

反应详情

EQUATION

反应方程式

HRID 21584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 1-methyl-5-(phenylmethoxy)-1H-indole-2-carboxylate (60.9 g, 197 mmol; Monge Vega A, et al., An. Ouim. 1976;72:267) in 550 mL of pyridine is cooled in ice and treated dropwise with a solution of pyridinium bromide perbromide (67.0 g, 209 mmol) in 200 mL of pyridine. The cooling bath is removed, and the mixture is stirred for 16 hours, then added to 4.0 L of cold water. The precipitated solid is filtered, washed with water, and recrystallized from ethyl acetate-hexane to give 58.4 g (76%) of product; mp 125-127° C.

WORKUP

后处理

  1. customThe cooling bath is removed
  2. additionadded to 4.0 L of cold water
  3. filtrationThe precipitated solid is filtered
  4. washwashed with water
  5. customrecrystallized from ethyl acetate-hexane