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Water → 1-[3-(1,3-Dimethyl-3,7-dihydro-1H-purine-2,6-dion-7-yl)-2-hydroxypropyl]-4-(3-phenylsulfonylpropyl)piperazine

HRID 1193491
ノート
印刷プレビュー

反応式

HRID 1193491 の反応式
[C:1]1([S:7]([CH2:10][CH2:11][CH2:12]Cl)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.Cl.[CH3:16][N:17]1[C:25](=[O:26])[C:24]2[N:23]([CH2:27][CH:28]([OH:36])[CH2:29][N:30]3[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]3)[CH:22]=[N:21][C:20]=2[N:19]([CH3:37])[C:18]1=[O:38].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:16][N:17]1[C:25](=[O:26])[C:24]2[N:23]([CH2:27][CH:28]([OH:36])[CH2:29][N:30]3[CH2:31][CH2:32][N:33]([CH2:12][CH2:11][CH2:10][S:7]([C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)(=[O:9])=[O:8])[CH2:34][CH2:35]3)[CH:22]=[N:21][C:20]=2[N:19]([CH3:37])[C:18]1=[O:38]
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 962WaterHCID 11430Potassium CarbonateHCID 11769949(3-Chloropropanesulfonyl)benzeneHCID 123426901-[3-(1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dion-7-yl)-2-hydroxypropyl]piperazine dihydrochloride

生成物 1

HCID 144575191-[3-(1,3-Dimethyl-3,7-dihydro-1H-purine-2,6-dion-7-yl)-2-hydroxypropyl]-4-(3-phenylsulfonylpropyl)piperazine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

0.13 Moles of 3-phenylsulfonyl-1-chloropropane were combined with 0.14 moles of 1-[3-(1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dion-7-yl)-2-hydroxypropyl]piperazine dihydrochloride and 0.3 moles potassium carbonate in 600 grams dimethylformamide. The mixture was stirred overnight at 60° C. After cooling, the reaction mixture was poured into water, extracted with CH2Cl2, washed with water, dried, and evaporated with gentle heating. The residue was recrystallized from ethanol to give the free base form of 1-[3-(1,3-Dimethyl-3,7-dihydro-1H-purine-2,6-dion-7-yl)-2-hydroxypropyl]-4-(3-phenylsulfonylpropyl)piperazine, m.p. 168° C. The dihydrochloride was obtained by adjunction with 12N hydrogen chloride solution as described in Example III, m.p. 190° C.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with CH2Cl2
  3. washwashed with water
  4. customdried
  5. customevaporated with gentle heating
  6. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-9c751f76c1df48deb0836f1ab11515f2
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04810706

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