HRID1816627

反应详情

EQUATION

反应方程式

HRID 1816627 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.8 g of methyl 2-amino-5-methyl-1,3-thiazole-4-carboxylate was dissolved in 30 ml methanol and 7 ml hydrobromic acid, followed by adding dropwise an aqueous solution of 1.2 g sodium nitrite thereinto under ice-cooling. After stirring the reaction solution under ice-cooling for 30 minutes, a solution, previously heated at 60° C., of 1.3 g cuprous bromide in 7 ml hydrobromic acid was added thereto, followed by stirring at 60° C. for 1 hour. The reaction solution was ice-cooled and water was-added, followed by extracting with diethyl ether. The organic layer was extracted with brine, dried over anhydrous magnesium sulfate and evaporated, to give 0.47 g of methyl 2-bromo-5-methyl-1,3-thiazole-4-carboxylate.

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. temperaturecooling for 30 minutes
  3. additionwas added
  4. stirringby stirring at 60° C. for 1 hour
  5. temperaturecooled
  6. extractionby extracting with diethyl ether
  7. extractionThe organic layer was extracted with brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customevaporated