HRID1258549

反应详情

EQUATION

反应方程式

HRID 1258549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred suspension of methyl 2-amino-5-methyl-1,3-thiazole-4-carboxylate (5 g, 29.03 mmol, 1 eq.) in 75 ml of MeCN, were added sodium bromide (5.97 g, 58.07 mmol, 2 eq.), Copper (I) bromide (6.08 g, 31.93 mmol, 1.1 eq.) and t-Butylnitrite (90%, 3.65 g, 31.93 mmol, 1.1 eq.). The reaction was slowly heated to 80° C. for 1 h and allowed to cool. MeCN was evaporated and 100 ml DCM were added to the residue. The crude was triturated, filtered through “celite” plug and washed with further 50 ml of EtOAc. The organic layers were combined, dried over MgSO4, and evaporated to give methyl 2-bromo-5-methyl-1,3-thiazole-4-carboxylate (3.91 g, 42% yield) as a yellow solid.

WORKUP

后处理

  1. temperatureto cool
  2. customMeCN was evaporated
  3. addition100 ml DCM were added to the residue
  4. customThe crude was triturated
  5. filtrationfiltered through “celite” plug
  6. washwashed with further 50 ml of EtOAc
  7. dry with materialdried over MgSO4
  8. customevaporated