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Benzene → HCID 19370330、化合物

HRID 129734
ノート
印刷プレビュー

反応式

HRID 129734 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 19370330HCID 19370330、化合物収率 75%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4ae16e94a4e6460f9a388a43b50f8ca0
出典データセット
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05470851

反応ノート

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