反应详情

A solution of 4-(2-methoxy-5-methylphenyl)-butyric acid (74 g, 0.36 mole), NaOAc (29.8 g, anhydrous), and glacial acetic acid (710 mL) was stirred under N2 at room temperature. as a solution of bromine (22 mL, 0.43 mole) and glacial acetic acid (185 mL) was added dropwise. The reaction mixture was stirred at room temperature for 20 hours. 10% aqueous sodium bisulfite (400 mL) was added and the solution was extracted with CH2Cl2. The combined extracts were washed with water, 10% aqueous sodium thiosulfate, water, saturated aqueous. NaCl, dried (MgSO4), filtered, and evaporated to yield 108 g brown solid which was recrystallized from hexane to yield 76 g white solid, (74%); m+ 286.

1. extractionthe solution was extracted with CH2Cl2
2. washThe combined extracts were washed with water, 10% aqueous sodium thiosulfate, water
3. dry with materialNaCl, dried (MgSO4)
4. filtrationfiltered
5. customevaporated