HRID239097

反应详情

EQUATION

反应方程式

HRID 239097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

238 μl tert.-butyl nitrite was added to 447 mg cupper (II) bromide in 50 mL acetonitrile. The reaction was stirred 10 min. at RT and then 270 mg 2-amino-4,5,7,8-tetrahydro-thiazolo[4,5-d]-azepine-6-carboxylic acid tert-butyl ester was added. The reaction was stirred 30 min. at 60° C. The reaction was purified by HPLC. The residue was dissolved in 10 mL dichlormethane and 10 mL trifluor acetic acid and stirred at RT for 1 h. The mixture was evaporated to give 112 mg of the desired product. Rt: 0.92 min (method I), (M+H)+: 233/235

WORKUP

后处理

  1. stirringThe reaction was stirred 30 min. at 60° C
  2. customThe reaction was purified by HPLC
  3. dissolutionThe residue was dissolved in 10 mL dichlormethane
  4. stirring10 mL trifluor acetic acid and stirred at RT for 1 h
  5. customThe mixture was evaporated