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Ethyl Acetate → 1-[Bis(4-fluorophenyl)methyl]-4-(3-fluorophenylcarbamoylmethyl)piperazine

HRID 1086244
ノート
印刷プレビュー

反応式

HRID 1086244 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1.[F:22][C:23]1[CH:24]=[C:25]([NH:29][C:30](=[O:33])[CH2:31]Cl)[CH:26]=[CH:27][CH:28]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>O1CCCC1.CN(C)C=O>[F:21][C:18]1[CH:19]=[CH:20][C:15]([CH:8]([C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=2)[N:9]2[CH2:10][CH2:11][N:12]([CH2:31][C:30](=[O:33])[NH:29][C:25]3[CH:26]=[CH:27][CH:28]=[C:23]([F:22])[CH:24]=3)[CH2:13][CH2:14]2)=[CH:16][CH:17]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 1529321-(Bis(4-fluorophenyl)methyl)piperazineHCID 23889312-chloro-N-(3-fluorophenyl)acetamide

生成物 1

HCID 151436391-[Bis(4-fluorophenyl)methyl]-4-(3-fluorophenylcarbamoylmethyl)piperazine

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

A mixture of 300 mg of 1-[bis(4-fluorophenyl)methyl]piperazine and 234 mg of N-(3-fluorophenyl)chloroacetamide was dissolved in 20 ml of a 1:1 by volume mixture of tetrahydrofuran and N,N-dimethylformamide, and 400 mg of anhydrous potassium carbonate were added to the solution. The reaction mixture was then stirred at 70° C. for 2 hours, after which ethyl acetate was added to it and the organic layer was separated. The organic layer was washed three times with water, and then dried over anhydrous magnesium sulfate. The solvent was removed by evaporation under reduced pressure. The residue was subjected to silica gel thin layer chromatography using a 2:1 by volume mixture of cyclohexane and ethyl acetate as the developing solvent, to give a purified 1-[bis(4-fluorophenyl)methyl]-4-(3-fluorophenylcarbamoylmethyl)piperazine.

後処理

  1. additionwere added to the solution
  2. customthe organic layer was separated
  3. washThe organic layer was washed three times with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed by evaporation under reduced pressure
  6. additionby volume mixture of cyclohexane and ethyl acetate as the developing solvent

出典と根拠

ORDレコード
ord-454b3d32b4264765961d03b4d51848f4
出典データセット
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05028610

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート