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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
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HRID 1193491 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c751f76c1df48deb0836f1ab11515f2
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04810706

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