Potassium Carbonate → 2-(4-(4-Diphenylmethyl-piperazin-1-yl)-3-hydroxy-butyl]isoindolin-1,3-dione

HRID 1070756

反応式

HRID 1070756 の反応式
[O:1]1[CH2:16][CH:2]1[CH2:3][CH2:4][N:5]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]1=[O:15].[CH:17]([N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[C:24]1([CH:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:30]2[CH2:31][CH2:32][N:33]([CH2:16][CH:2]([OH:1])[CH2:3][CH2:4][N:5]3[C:13](=[O:14])[C:12]4[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=4)[C:6]3=[O:15])[CH2:34][CH2:35]2)[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 70048BenzhydrylpiperazineHCID 3394332-[2-(oxiran-2-yl)ethyl]-2,3-dihydro-1H-isoindole-1,3-dione

生成物 1

HCID 223976852-(4-(4-Diphenylmethyl-piperazin-1-yl)-3-hydroxy-butyl]isoindolin-1,3-dione

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5 g (˜25 mmol) 2-(3,4-epoxybutyl)-isoindolin-1,3-dione, 7.5 g (30 mmol) benzhydrylpiperazine and 3.5 g (25 mmol) potassium carbonate are stirred in DMF for 6 hours 80° C. After cooling, the reaction mixture is filtered and concentrated under vacuum. The residue is taken up in 300 ml acetic acid ethyl ester and washed three times each with 20 ml water. The organic phase is dried over sodium sulfate and the solvent is removed under vacuum. The residue is chromatographically purified over silica gel with CHCl3/CH3OH.

後処理

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture is filtered
  3. concentrationconcentrated under vacuum
  4. washwashed three times each with 20 ml water
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. customthe solvent is removed under vacuum
  7. customThe residue is chromatographically purified over silica gel with CHCl3/CH3OH

出典と根拠

ORDレコード
ord-74029f5adc144f849d7c7dffec248640
出典データセット
uspto-grants-2005_06
特許番号
US06903118B1

関連ノート

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