Water → 1-Acetyl-4-(3-hydroxyphenyl)piperazine

HRID 1156290노트

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HRID 1156290 반응식
Br.Br.[N:3]1([C:9]2[CH:10]=[C:11]([OH:15])[CH:12]=[CH:13][CH:14]=2)[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.O.C(=O)([O-])O.[Na+].[C:22](OC(=O)C)(=[O:24])[CH3:23]>ClC(Cl)Cl>[C:22]([N:6]1[CH2:5][CH2:4][N:3]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([OH:15])[CH:10]=2)[CH2:8][CH2:7]1)(=[O:24])[CH3:23]

참가 물질

6

반응물 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 198170793-(1-Piperazinyl)phenol dihydrobromide

생성물 1

HCID 128548521-Acetyl-4-(3-hydroxyphenyl)piperazine수율 70%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
10 °C

실험 절차

To a stirred solution of 80 parts of 3-(1-piperazinyl)phenol dihydrobromide in 360 parts of water and 180 parts of trichloromethane are added portionwise 42 parts of sodium hydrogen carbonate at 10° C. Then there are added dropwise, during a 15 minutes-period, 26 parts of acetic acid anhydride while cooling at 10° C. Upon completion, stirring is continued for 3 hours at room temperature. The precipitated product is filtered off, washed with water and crystallized from 2-propanol, yielding 37 parts (70%) of 1-acetyl-4-(3-hydroxyphenyl)piperazine; mp. 186.1° C.

후처리

  1. filtrationThe precipitated product is filtered off
  2. washwashed with water
  3. customcrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-fc4ef5ce7c7a40998b9fbc3b3ec86ce3
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04335125

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