HRID839922

反应详情

EQUATION

反应方程式

HRID 839922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 930 mg of ethyl 2-amino-4-thiazolyl-acetate, 25 ml of dry chloroform, 0.8 ml of triethylamine and 1.65 g of trityl chloride was stirred for 3 hours and then 3 ml of N hydrochloric acid and 5 ml of water were added thereto. The mixture was stirred and decanted and 5 ml of N hydrochloric acid and 5 ml of water were again added. The mixture was decanted and the organic phase was dried and evaporated to dryness. The residue was added to 10 ml of dioxane and 6 ml of N sodium hydroxide and the mixture was stirred at 50° C and then stood overnight at room temperature. The mixture was evaporated to dryness and the residue was diluted with water. The solution was washed with ether and was acidified with 0.5 ml of acetic acid. The mixture was allowed to crystallize and was then vacuum filtered to obtain 1.33 g of 2-tritylamino-4-thiazolyl-acetic acid which after empasting with ether melted at 220° C.

WORKUP

后处理

  1. stirringThe mixture was stirred
  2. customdecanted
  3. addition5 ml of N hydrochloric acid and 5 ml of water were again added
  4. customThe mixture was decanted
  5. customthe organic phase was dried
  6. customevaporated to dryness
  7. additionThe residue was added to 10 ml of dioxane and 6 ml of N sodium hydroxide
  8. stirringthe mixture was stirred at 50° C
  9. waitstood overnight at room temperature
  10. customThe mixture was evaporated to dryness
  11. additionthe residue was diluted with water
  12. washThe solution was washed with ether
  13. customto crystallize
  14. filtrationvacuum filtered