HRID1506025
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
A solution of (6-methoxy-4-iodo-pyridin-3-yl)-carbamic acid tert-butyl ester (18 g, 51 mmol) in DCM (50 mL) and TFA (50 mL) was stirred at ambient temperature for 1 h and then evaporated in vacuo. The resultant residue was treated with saturated aqueous sodium hydrogen carbonate solution (25 mL), diluted with water (100 mL) and extracted into ethyl acetate (2×100 mL). The organic layer was separated, dried over sodium sulfate, filtered and evaporated in vacuo to afford the title compound as a brown foam (10 g, 60%).
WORKUP
后处理
- customevaporated in vacuo
- additionThe resultant residue was treated with saturated aqueous sodium hydrogen carbonate solution (25 mL)
- additiondiluted with water (100 mL)
- extractionextracted into ethyl acetate (2×100 mL)
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated in vacuo