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Ethyl cyclohexanoate → 3,7-dihydro-3-methyl-7-([5-cyclohexyl-1,2,4-oxadiazole-3-yl]methyl)-1H-purine-2,6-dione

HRID 1904905
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HRID 1904905 반응식
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][C:12](=[N:14][OH:15])[NH2:13])[C:6]=2[C:5](=[O:16])[NH:4][C:3]1=[O:17].[Na].[CH:19]1([C:25](OCC)=O)[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1>C(O)C>[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][C:12]3[N:13]=[C:25]([CH:19]4[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]4)[O:15][N:14]=3)[C:6]=2[C:5](=[O:16])[NH:4][C:3]1=[O:17]
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참가 물질

5

반응물 3

HCID 18686Ethyl cyclohexanoateHCID 5360545SodiumHCID 537117962-(3-Methyl-xanthine-7-yl)acetamidoxime

생성물 1

HCID 147484583,7-dihydro-3-methyl-7-([5-cyclohexyl-1,2,4-oxadiazole-3-yl]methyl)-1H-purine-2,6-dione수율 76%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of 2.38 g of 2-(3-methyl-xanthine-7-yl)acetamidoxime in 25 ml of ethanol is admixed with a solution of 0.46 g of metallic sodium in 25 ml of ethanol and 3.02 g of ethyl cyclohexane carboxylate. The reaction mixture is heated to boiling under stirring for 10 hours, then evaporated. The residue is admixed with water and the pH is adjusted to 7. The precipitate is crystallized from aqueous ethanol. Thus 2.51 g of 3,7-dihydro-3-methyl-7-([5-cyclohexyl-1,2,4-oxadiazole-3-yl]methyl)-1H-purine-2,6-dione are obtained, m.p.: 245°-248° C.

후처리

  1. temperatureThe reaction mixture is heated
  2. customevaporated
  3. customThe precipitate is crystallized from aqueous ethanol

출처 및 근거

ORD 기록
ord-21fc83428b274d28a216df1e6e05e9c6
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04840949

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