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Chloroacetone → HCID 11558165、化合物

HRID 856015
ノート
印刷プレビュー

反応式

HRID 856015 の反応式
C(=O)([O-])[O-].[K+].[K+].C(N(C(C)C)C(C)C)C.Cl[CH2:17][C:18](=[O:20])[CH3:19].[N:21]1([C:27]([O:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[O:28])[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>C(#N)C>[O:20]=[C:18]([CH3:19])[CH2:17][N:24]1[CH2:23][CH2:22][N:21]([C:27]([O:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[O:28])[CH2:26][CH2:25]1
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 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 643495Benzyl piperazine-1-carboxylate

生成物 1

HCID 11558165HCID 11558165、化合物収率 88%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Potassium carbonate (1.27 g, 9.22 mmol), N-ethyldiisopropylamine (0.80 ml, 4.61 mmol), and chloroacetone (1.22 ml, 13.83 mmol) were added to a solution of benzyl piperazine-1-carboxylate (2.03 g, 90.22 mmol) in acetonitrile(20 ml), and the mixture was heated under reflux for 2 hours. The insoluble substances were removed by filtration and washed with ethyl acetate. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography(methylene chloride/methanol=100/1) to afford benzyl 4-(2-oxopropyl)piperazine-1-carboxylate (2.24 g, yield 88%) as a pale yellow oil.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. customThe insoluble substances were removed by filtration
  4. washwashed with ethyl acetate
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography(methylene chloride/methanol=100/1)

出典と根拠

ORDレコード
ord-3fae510a45ed4a9f9af3666d7a866882
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262212B2

反応ノート

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