反应详情

Boron trifluoride dimethyl sulfide (10 μL, 80 μmol) was added at room temperature to a stirred solution of methyl-N-[3,5-dichloro-4-(2-bromo-4-methoxy-5-isopropylphenoxy)benzoyl]glycine (1.0 mg, 2.0 μmol) and dichloromethane (0.50 mL). The reaction mixture was stirred at room temperature for 8 hours and then treated with ice-water, extracted with ethyl acetate and washed with water. The organic phase was dried over sodium sulphate and concentrated to give a light yellow solid. The solid was purified on column (MPLC, silica gel, chloroform/methanol/acetic acid, gradient elution from 1/0/0 to 95/5/0.5) to give 0.90 mg (94%) of N-[3,5-dichloro-4-(2-bromo-4-hydroxy-5-isopropylphenoxy)benzoyl]glycine. LC-MS (ES−1): m/z 476.

1. extractionextracted with ethyl acetate
2. washwashed with water
3. dry with materialThe organic phase was dried over sodium sulphate
4. concentrationconcentrated
5. customto give a light yellow solid
6. customThe solid was purified on column (MPLC, silica gel, chloroform/methanol/acetic acid, gradient elution from 1/0/0 to 95/5/0.5)