反应详情

To a slurry of 3-(4-methoxybenzamido)-4-hydroxy-α-(tert.butylaminomethyl)benzylalcohol hydrochloride (0.5 g, 0.0013 mole) in glacial acetic acid (5 ml) a glacial acetic acid/chlorine solution (11.86 ml) containing 0.0898 g (0.0013 mole) of chlorine was added at room temperature with stirring during 10 minutes. The mixture was kept with continued stirring for 24 hours at room temperature, whereafter insoluble substance was filtered off, washed with ether, and air-dried (160 mg) (32%), melting point 196° - 199° C. 80 mg of the crude product was recrystallized from methanol (2 ml) (insoluble substance was filtered off). The yield of the analytically pure 3-(4-methoxybenzamido)-4-hydroxy-5-chloro-α-(tert.butylaminomethyl)benzylalcohol hydrochloride was 50 mg (20%), m.p. 205° - 206° C.

1. additionwas added at room temperature
2. stirringwith continued stirring for 24 hours at room temperature, whereafter insoluble substance
3. filtrationwas filtered off
4. washwashed with ether
5. customair-dried (160 mg) (32%), melting point 196° - 199° C
6. custom80 mg of the crude product was recrystallized from methanol (2 ml) (insoluble substance was filtered off)