反应详情

A mixture of water (50 ml) and 29.5 g of sodium thiosulfate pentahydrate was added to o-(chloromethyl)benzoic acid methyl ester 20 g, and stirred for 5 hours at 50˜55° C. 300 ml of acetic acid was added and then excess of chlorine gas for 3 hours was infused, while maintaining the internal temperature of reactor at 5˜10° C. The reaction mixture was further stirred for 1 hour at the same temperature. Excess of chlorine gas was removed via infusion of nitrogen gas and with the addition of ice water (300 ml), stirred for 30 minutes. A solid, so formed, was filtered with a cold water and dried to afford 22.4 g of desired compound (yield 83%) as a white solid.

1. temperaturewhile maintaining the internal temperature of reactor at 5˜10° C
2. stirringThe reaction mixture was further stirred for 1 hour at the same temperature
3. customExcess of chlorine gas was removed via infusion of nitrogen gas and with the addition of ice water (300 ml)
4. stirringstirred for 30 minutes
5. customA solid, so formed
6. filtrationwas filtered with a cold water
7. customdried