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

HRID 1262524
ノート
印刷プレビュー

反応式

HRID 1262524 の反応式
[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]
参加物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 6228DimethylformamideHCID 8083MorpholineHCID 24386Thionyl ChlorideHCID 155873004-(1,3-diethyl-2,3,6,7-tetrahydro-2,6-dioxo-1H-purin-8-yl)benzenesulfonic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

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).

後処理

  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°

出典と根拠

ORDレコード
ord-5e5d18ea53c3457f870e52e93de46733
出典データセット
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04452788

反応ノート

読み込み中…

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