HRID418343
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
Suspended CuBr2 (905 mg, 4.05 mmol) in 5 mL of DMF and added i-butylnitrite (0.57 mL), 4.86 mmol). To this was added 2-amino-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid tert-butyl ester (860 mg, 3.36 mmol) and the mixture was stirred for 2 h at 60° C. LC-MS analysis indicated the desired bromide. Concentrated the mixture to a brown-red residue. Dissolved the residue in CH2Cl2 and purified via SiO2 chromatography (EtOAc/hexanes 0-20%) to give 650 mg of 2-bromo-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid tert-butyl ester.
WORKUP
后处理
- concentrationConcentrated the mixture to a brown-red residue
- dissolutionDissolved the residue in CH2Cl2
- custompurified via SiO2 chromatography (EtOAc/hexanes 0-20%)