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Benzene → HCID 19370330, 화합물

HRID 129734
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HRID 129734 반응식
[CH3:1][C:2]([OH:15])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl[CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][N:22]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:21][CH2:20]1.[NH2-].[Na+].C1C=CC=CC=1>O>[CH2:28]([O:27][C:25]([N:22]1[CH2:21][CH2:20][N:19]([CH2:18][CH2:17][O:15][C:2]([C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH3:1])[CH2:24][CH2:23]1)=[O:26])[CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 241BenzeneHCID 24533Sodium amideHCID 690311,1-DiphenylethanolHCID 201594Ethyl 4-(2-chloroethyl)piperazine-1-carboxylate

생성물 1

HCID 19370330HCID 19370330, 화합물수율 75%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1.8 g (9.1 mmole) of α-methylbenzhydrol, 2.0 g (9.1 mmole) of 1-(2-chloroethyl)-4-(ethoxycarbonyl)piperazine, 0.36 g (9.2 mmole) of sodium amide and 20 ml of benzene was heated under reflux overnight. At the end of this time, water was poured onto the reation mixture, and the mixture was extracted with ethyl acetate. The solvent was then removed from the mixture by distillation under reduced pressure, and the residue was subjected to column chromatography through silica gel, using a 1:1 by volume mixture of ethyl acetate and hexane as the eluent, to obtain 2.5 g (yield 75%) of the title compound as an oil.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. extractionthe mixture was extracted with ethyl acetate
  4. customThe solvent was then removed from the mixture by distillation under reduced pressure
  5. additionby volume mixture of ethyl acetate and hexane as the eluent

출처 및 근거

ORD 기록
ord-4ae16e94a4e6460f9a388a43b50f8ca0
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05470851

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