HRID239102
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
PROCEDURE
实验过程
39 g calcium carbonate and 36.8 g phenyl chloroformate in 250 mL THF was added to a stirred solution of 50 g 2-amino-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid tert-butyl ester in 1 L THF. The reaction mixture was allowed to stir for 15 h at RT. The reaction mixture was filtered through silica gel and the filtrate was concentrated under reduced pressure. The residue was diluted with water and extracted with ethyl acetate and the organic layer was dried over magnesium sulfate. The organic layer was concentrated under reduced pressure. The residue was washed with 20% ethyl acetate in hexane to give 60 g of the desired product.
WORKUP
后处理
- filtrationThe reaction mixture was filtered through silica gel
- concentrationthe filtrate was concentrated under reduced pressure
- additionThe residue was diluted with water
- extractionextracted with ethyl acetate
- dry with materialthe organic layer was dried over magnesium sulfate
- concentrationThe organic layer was concentrated under reduced pressure
- washThe residue was washed with 20% ethyl acetate in hexane