HRID860959
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
Boron trifluoride dimethyl sulfide (1.0 mL) was added at room temperature to a stirred solution of methyl-N-[3,5-dichloro-4-(3-chloro-5-isopropyl-4-methoxyphenoxy)benzoyl]glycine (90 mg) and dichloromethane (10 mL). The reaction mixture was stirred at room temperature for 24 hours, poured out in water and extracted with ethyl acetate (3×30 mL). The combined organic phases were washed with water (4×20 mL), concentrated and the resulting residue purified on column (silica gel, chloroform/methanol/acetic acid 94:6:0.65). This gave 53 mg (63%) of N-[3,5-dichloro-4-(3-chloro-4-hydroxy-5-isopropylphenoxy)benzoyl]glycine. LC-MS (ES+1): m/z 434.
WORKUP
后处理
- extractionextracted with ethyl acetate (3×30 mL)
- washThe combined organic phases were washed with water (4×20 mL)
- concentrationconcentrated
- customthe resulting residue purified on column (silica gel, chloroform/methanol/acetic acid 94:6:0.65)