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Dimethylformamide → 1,3-Diethyl-8-[4-(morpholine-4-sulfonyl)-phenyl]-3,7-dihydro-purine-2,6-dione

HRID 1262524
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HRID 1262524 반응식
[CH2:1]([N:3]1[C:11](=[O:12])[C:10]2[NH:9][C:8]([C:13]3[CH:18]=[CH:17][C:16]([S:19](O)(=[O:21])=[O:20])=[CH:15][CH:14]=3)=[N:7][C:6]=2[N:5]([CH2:23][CH3:24])[C:4]1=[O:25])[CH3:2].CN(C)C=O.S(Cl)(Cl)=O.[NH:35]1[CH2:40][CH2:39][O:38][CH2:37][CH2:36]1>O>[CH2:1]([N:3]1[C:11](=[O:12])[C:10]2[NH:9][C:8]([C:13]3[CH:14]=[CH:15][C:16]([S:19]([N:35]4[CH2:40][CH2:39][O:38][CH2:37][CH2:36]4)(=[O:20])=[O:21])=[CH:17][CH:18]=3)=[N:7][C:6]=2[N:5]([CH2:23][CH3:24])[C:4]1=[O:25])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8083MorpholineHCID 24386Thionyl ChlorideHCID 155873004-(1,3-diethyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)benzenesulfonic acid

생성물 1

HCID 155873081,3-Diethyl-8-[4-(morpholine-4-sulfonyl)-phenyl]-3,7-dihydro-purine-2,6-dione수율 54.2%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

A mixture of 4-(1,3-diethyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)benzenesulfonic acid (5.0 g, 0.014 moles) and N,N-dimethylformamide (150 ml) is cooled to 0° and treated with thionyl chloride (3.3 g, 0.027 moles). When the addition is complete, the reaction mixture is permitted to warm to ambient temperature and stirred vigorously until a thick slurry results. To this slurry is added morpholine (20 g, 0.23 moles) in one portion. The resulting slurry is stirred one hour and poured into two liters of water. The resulting suspension is filtered, triturated with ethanol, and dried at 68° to yield 3.29 grams of 4-[[4-(1,3-diethyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)phenyl]sulfonyl]morpholine, mp 354°-355° C.(d).

후처리

  1. temperatureis cooled to 0°
  2. additionWhen the addition
  3. customresults
  4. stirringThe resulting slurry is stirred one hour
  5. filtrationThe resulting suspension is filtered
  6. customtriturated with ethanol
  7. customdried at 68°

출처 및 근거

ORD 기록
ord-5e5d18ea53c3457f870e52e93de46733
출처 데이터셋
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04452788

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