반응 #1817035

반응 방정식

1-(3'-hydroxyphenyl)-2-amino-ethanol hydrochloride

water

water

cyclohexane

→

2-(3'-HYDROXYPHENYL)-1-OXA-4-AZASPIRO[4,5]DECANE

용매

benzene

benzene

반응 조건

후처리

1. 1
   workup.ADDITIONA suspension of 20 g
2. 2
   기타equipped with a dropping funnel
3. 3
   기타Above a temperature of 80° C.
4. 4
   workup.DISTILLATIONis distilled of azeotropically
5. 5
   기타is, at the finish, about 130° C
6. 6
   온도After cooling
7. 7
   기타the crystalline reaction product is separated off
8. 8
   기타collected on a frit
9. 9
   기타There is obtained 20.3 g
10. 10
    기타After recrystallization from isopropanol/ethyl acetate
11. 11
    기타the product is obtained in the form of colorless crystals with a melting point of 138° - 139° C.

실험 절차

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.

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