Formic Acid → 1H-Purine-2,6-dione, 3,7-dihydro-3-butyl-

HRID 1381856

반응식

HRID 1381856 반응식
[CH2:1]([N:5]1[C:10]([NH2:11])=[C:9]([NH2:12])[C:8](=[O:13])[NH:7][C:6]1=[O:14])[CH2:2][CH2:3][CH3:4].[CH:15](O)=O>>[CH2:1]([N:5]1[C:10]2[N:11]=[CH:15][NH:12][C:9]=2[C:8](=[O:13])[NH:7][C:6]1=[O:14])[CH2:2][CH2:3][CH3:4]

참가 물질

3

반응물 2

HCID 284Formic AcidHCID 10584108HCID 10584108, 화합물

생성물 1

HCID 2186671H-Purine-2,6-dione, 3,7-dihydro-3-butyl-

실험 절차

A solution of 36.6 g of 1-butyl-5,6-diamino-2,4-(1H,3H)-pyrimidinedione (X) in 100 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 42.9 g (not dried). (XI). The amide (XI) was refluxed in 100 ml of 2N NaOH for 2 hours and then neutralized with 5N HCl. The crystals were filtered off and washed with ethanol. Yield 28.4 g (74%) (XII), NMR. ##STR9##

후처리

  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. customYield 42.9 g (not dried)
  6. temperatureThe amide (XI) was refluxed in 100 ml of 2N NaOH for 2 hours
  7. filtrationThe crystals were filtered off
  8. washwashed with ethanol

출처 및 근거

ORD 기록
ord-fc908581e83c42c195d17778a07399b8
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804664

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