HRID1723684
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
To a solution of 6-acetyl-2-(2-chlorophenylamino)-3,4-difluorobenzoic acid (50 mg, 0.15 mmol) and hydroxylamine hydrochloride (11 mg, 0.15 mmol) in MeOH-H2O (1 mL/0.5 mL) was added TEA (0.022 mL, 0.15 mmol) at room temperature. The resulting mixture was stirred for 16 hours at room temperature. The reaction mixture was diluted with EtOAc and washed with water. The organic layer was dried over MgSO4, filtered and concentrated in vacuo to give the crude material that was purified by silica gel flash column chromatography (100% CH2Cl2) to afford the desired product (26.8 mg, 54%).
WORKUP
后处理
- washwashed with water
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give the crude material that
- customwas purified by silica gel flash column chromatography (100% CH2Cl2)