HRID1168078

反应详情

EQUATION

反应方程式

HRID 1168078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 335 mg of 4-[2-(Benzo[b]thiophene-4-yloxy)-ethyl]-5-methyl-2-phenyl-oxazole (1 mmol) and 110 mg of Trioxane (3.6 mmol) in 15 ml dichloromethane was treated with 2 ml of 37% HCl solution and saturated for 10 min with HCl gas and reacted at 2° C. for 23 h. The resulting mixture was extracted wich 10% sodium carbonate solution and water and evaporated to dryness. Digestion with tert. butyl methylether at room temperature left a light brown residue (0.11 g) consisting of 4-[2-(7-Chloromethyl-benzo[b]thiophen-4-yloxy)-ethyl]-5-methyl-2-phenyl-oxazole with a m.p. of 144-145° C.

WORKUP

后处理

  1. customreacted at 2° C. for 23 h
  2. extractionThe resulting mixture was extracted wich 10% sodium carbonate solution and water
  3. customevaporated to dryness
  4. waitDigestion with tert. butyl methylether at room temperature left a light brown residue (0.11 g)