HRID77338

反应详情

EQUATION

反应方程式

HRID 77338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
28 °C

PROCEDURE

实验过程

To 8.64 g (0.36 mole) of sodium hydride in toluene (250 ml) was added 2-hydroxymethyl-8-phenethyl-1,4-dioxa-8-azaspiro[4,5]decane (compound 1.50 gm, 0.18 mole) in toluene (350 ml) with stirring at 28° C. The phase transfer catalyst tetrabutylammonium bromide TBAB 2 gm was added and 31 gm of 2-chloro-5-chloromethylthiazole in toluene (225 ml) was then added drop wise at 10° C. and the reaction mixture was refluxed for 15 hrs. The reaction mixture was washed with water and the product was extracted with methylene chloride 100 ml. The solvent was distilled off to get thick dark colored liquid. The yield of the product was 85%.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 15 hrs
  2. washThe reaction mixture was washed with water
  3. extractionthe product was extracted with methylene chloride 100 ml
  4. distillationThe solvent was distilled off
  5. customto get thick dark colored liquid