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Dimethyl Sulfoxide → 5-[5-(4-Phenyl-1-piperazinyl)valeryl]-2-benzyloxy-benzamide

HRID 65208
ノート
印刷プレビュー

反応式

HRID 65208 の反応式
Cl[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:9]=[CH:10][C:11]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:12]([CH:16]=1)[C:13]([NH2:15])=[O:14])=[O:7].[C:25]1([N:31]2[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(=O)([O-])[O-].[Na+].[Na+].CS(C)=O>O>[C:25]1([N:31]2[CH2:36][CH2:35][N:34]([CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]3[CH:9]=[CH:10][C:11]([O:17][CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)=[C:12]([CH:16]=3)[C:13]([NH2:15])=[O:14])=[O:7])[CH2:33][CH2:32]2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=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

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 70961-PhenylpiperazineHCID 10340Sodium CarbonateHCID 202339675-(5-Chlorovaleryl)-2-benzyloxy-benzamide

生成物 1

HCID 202339515-[5-(4-Phenyl-1-piperazinyl)valeryl]-2-benzyloxy-benzamide収率 84.3%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
90 °C

実験手順

A mixture of 2 g of 5-(5-chlorovaleryl)-2-benzyloxy-benzamide, 1 g of 1-phenylpiperazine, 0.6 g of sodium carbonate and 10 ml of dimethyl sulfoxide was heated at 90° C. for 6 hours while stirring. After the reaction was finished, water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with water saturated with sodium chloride, dried over anhydrous sodium sulfate and concentrated. The thus produced residue was dissolved in acetone and concentrated hydrochloric acid in an amount of 2 equivalents was added thereto to produce crystals. The crystals were filtered off to obtain 2.3 g of 5-[5-(4-phenyl-1-piperazinyl)valeryl]-2-benzyloxy-benzamide (yield: 73%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water saturated with sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. dissolutionThe thus produced residue was dissolved in acetone
  6. additionconcentrated hydrochloric acid in an amount of 2 equivalents was added
  7. customto produce crystals
  8. filtrationThe crystals were filtered off

出典と根拠

ORDレコード
ord-cfbb51c4de9446b3ae8f6ac9ea57ff96
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04613598

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