反应详情

To a stirred mixture of lithium aluminium hydride (12 g) and dry diethyl ether (350 ml), a solution of methyl 3-amino-4-benzyl-5-sulfamylbenzoate (30 g) in dry pyridine (300 ml) is dropwise added during 1-1.5 hours. After additional stirring for 3 hours, the mixture is cooled and ethyl acetate (25 ml) followed by water (50 ml) are very cautiously added dropwise. After stirring for a further 30 minutes, the solids are collected by filtration and dried in air. The filter cake is treated with hot 4 N hydrochloric acid (about 500 ml) to dissolve inorganic material. After cooling 3-amino-4-benzyl-5-sulfamylbenzyl alcohol is collected by filtration and dried in air. After recrystallization from aqueous ethanol it is obtained with a melting point of 159°-161° C.

1. temperaturethe mixture is cooled
2. additionare very cautiously added dropwise
3. stirringAfter stirring for a further 30 minutes
4. filtrationthe solids are collected by filtration
5. customdried in air
6. additionThe filter cake is treated with hot 4 N hydrochloric acid (about 500 ml)
7. dissolutionto dissolve inorganic material
8. temperatureAfter cooling 3-amino-4-benzyl-5-sulfamylbenzyl alcohol
9. filtrationis collected by filtration
10. customdried in air
11. customAfter recrystallization from aqueous ethanol it
12. customis obtained with a melting point of 159°-161° C.