Formic Acid → 1H-Purine-2,6-dione, 3,7-dihydro-3-(2-methylpropyl)-

HRID 1381858ノート

反応式

HRID 1381858 の反応式
[NH2:1][C:2]1[C:3](=[O:14])[NH:4][C:5](=[O:13])[N:6]([CH2:9][CH:10]([CH3:12])[CH3:11])[C:7]=1[NH2:8].[CH:15](O)=O>>[CH3:12][CH:10]([CH3:11])[CH2:9][N:6]1[C:7]2[N:8]=[CH:15][NH:1][C:2]=2[C:3](=[O:14])[NH:4][C:5]1=[O:13]

参加物

3

反応物 2

HCID 284Formic AcidHCID 105841095,6-Diamino-1-(2-methylpropyl)-1,2,3,4-tetrahydropyrimidine-2,4-dione

生成物 1

HCID 30485051H-Purine-2,6-dione, 3,7-dihydro-3-(2-methylpropyl)-

実験手順

A solution of 24.2 g of 5,6-diamino-1-(2-methylpropyl)-2,4-(1H,3H)-pyrimidinedione (XVI) in 60 ml of formic acid was refluxed for 2 hours. The hot solution was filtered and 30 ml of chloroform was added and ether was then added slowly. The received crystals were filtered off. Yield 17.8 g (XVII). The amide (XVII) was refluxed in 50 ml of 2N NaOH for 2 hours and then neutralized with 5N HCl. The crystals were filtered off and recrystallized from ethanol. Yield 11.6 g (46%), NMR. ##STR10##

後処理

  1. filtrationThe hot solution was filtered
  2. addition30 ml of chloroform was added
  3. additionether was then added slowly
  4. filtrationThe received crystals were filtered off
  5. temperatureThe amide (XVII) was refluxed in 50 ml of 2N NaOH for 2 hours
  6. filtrationThe crystals were filtered off
  7. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-a3263eb1af304faa8b53f6a5cfa04a29
出典データセット
uspto-grants-1989_02
特許番号
US04804664

反応ノート

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