Ethanol → CH-13584

HRID 1904903노트

반응식

HRID 1904903 반응식
[CH3:1][CH2:2][O-:3].[Na+].[Na].C(O)C.[CH3:9][N:10]1[C:18]2[N:17]=[CH:16][N:15]([CH2:19][C:20](=[N:22]O)[NH2:21])[C:14]=2[C:13](=[O:24])[NH:12][C:11]1=[O:25]>C(OCC)(=O)C>[CH3:9][N:10]1[C:18]2[N:17]=[CH:16][N:15]([CH2:19][C:20]3[N:22]=[C:2]([CH3:1])[O:3][N:21]=3)[C:14]=2[C:13](=[O:24])[NH:12][C:11]1=[O:25]

참가 물질

6

반응물 4

HCID 702EthanolHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 537117962-(3-Methyl-xanthine-7-yl)acetamidoxime

생성물 1

HCID 163975CH-13584

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of a sodium ethylate solution prepared from 6.76 g of metallic sodium and 290 ml of anhydrous ethanol, 35 g of 2-(3-methyl-xanthine-7-yl)-acetamidoxime and 43.0 g of ethyl acetate is heated to boiling under stirring for 4 hours. The hot reaction mixture is filtered, the filtrate is evaporated in vacuo and the residue is dissolved in 200 ml of water. The pH of the solution is adjusted to 7 by adding 10% hydrochloric acid, the precipitate is filtered by suction and crystallized twice from water. Thus, 18.0 g of 3,7-dihydro-3-methyl-7-([5-methyl-1,2,4-oxadiazole-3-yl]-methyl)-1H-purine-2,6-dione are obtained, m.p.: 262°-264° C.

후처리

  1. temperatureis heated
  2. filtrationThe hot reaction mixture is filtered
  3. customthe filtrate is evaporated in vacuo
  4. dissolutionthe residue is dissolved in 200 ml of water
  5. additionby adding 10% hydrochloric acid
  6. filtrationthe precipitate is filtered by suction
  7. customcrystallized twice from water

출처 및 근거

ORD 기록
ord-46c8110c31fd40d699156ebc59ba83ea
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04840949

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