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Benzoic Acid → 3,9-Dihydro-8-phenyl-1,3-dipropyl-1H-purine-2,6-dione

HRID 622082
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HRID 622082 반응식
[CH2:1]([N:4]1[C:11]([NH2:12])=[C:10]([NH2:13])[C:8](=[O:9])[N:7]([CH2:14][CH2:15][CH3:16])[C:5]1=[O:6])[CH2:2][CH3:3].[C:17](O)(=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>CO>[CH2:14]([N:7]1[C:8](=[O:9])[C:10]2[NH:13][C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[N:12][C:11]=2[N:4]([CH2:1][CH2:2][CH3:3])[C:5]1=[O:6])[CH2:15][CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 243Benzoic AcidHCID 50986055,6-Diamino-1,3-dipropyl-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 1287843,9-Dihydro-8-phenyl-1,3-dipropyl-1H-purine-2,6-dione수율 77%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1,3-dipropyl-5,6-diaminouracil (0.01 mol) was dissolved in 30 ml methanol, followed by 0.01 mol of benzoic acid and then 0.01 mol of DICD. The solution was stirred for 30 min at room temperature, filtered, and washed with a small amount of methanol. The solid was boiled for ten minutes in 2.5N KOH, filtered hot, and the liquid neutralized with concentrated HCl. The solid was collcted by filtration, washed with water, redissolved in 100 ml with a minimum amount of KOH, precipitated by neutralization with HCl, filtered, washed with water, and dried. The product was identified by chemical ionization mass spectrometry and elemental Analysis. Yield 77%.

후처리

  1. filtrationfiltered
  2. washwashed with a small amount of methanol
  3. waitThe solid was boiled for ten minutes in 2.5N KOH
  4. filtrationfiltered hot
  5. filtrationThe solid was collcted by filtration
  6. washwashed with water
  7. dissolutionredissolved in 100 ml with a minimum amount of KOH
  8. customprecipitated by neutralization with HCl
  9. filtrationfiltered
  10. washwashed with water
  11. customdried

출처 및 근거

ORD 기록
ord-2fdb30d8c4e14c329e0fc9b5b224ddba
출처 데이터셋
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04769377

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