反应详情

A suspension of 20 g. of 1-(3'-hydroxyphenyl)-2-amino-ethanol hydrochloride in 100 ml. of cyclohexane is heated, while stirring vigorously, in a three-necked flask equipped with a dropping funnel, water separator, and thermometer. Above a temperature of 80° C., up to 100 ml. of benzene are added dropwise in such a manner so that the water of reaction formed together with the benzene is distilled of azeotropically. The temperature of the flask contents is, at the finish, about 130° C. After cooling, the crystalline reaction product is separated off, digested with benzene, and collected on a frit. There is obtained 20.3 g. (71.5% of theory) of 2-(3'-hydroxyphenyl)-1-oxa-4-azospiro[4,5]decane hydrochloride. After recrystallization from isopropanol/ethyl acetate, the product is obtained in the form of colorless crystals with a melting point of 138° - 139° C.

1. additionA suspension of 20 g
2. customequipped with a dropping funnel
3. customAbove a temperature of 80° C.
4. distillationis distilled of azeotropically
5. customis, at the finish, about 130° C
6. temperatureAfter cooling
7. customthe crystalline reaction product is separated off
8. customcollected on a frit
9. customThere is obtained 20.3 g
10. customAfter recrystallization from isopropanol/ethyl acetate
11. customthe product is obtained in the form of colorless crystals with a melting point of 138° - 139° C.