Diethyl Ether → 6-Hydroxy-8-methyl-3-(2-methylpropyl)-3,9-dihydro-2H-purin-2-one

HRID 236305노트

반응식

HRID 236305 반응식
[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].C(Cl)(Cl)Cl.[CH3:19][CH2:20]OCC>C(O)(=O)C>[CH3:19][C:20]1[NH:1][C:2]2[C:3](=[O:14])[NH:4][C:5](=[O:13])[N:6]([CH2:9][CH:10]([CH3:11])[CH3:12])[C:7]=2[N:8]=1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 6212ChloroformHCID 105841095,6-Diamino-1-(2-methylpropyl)-1,2,3,4-tetrahydropyrimidine-2,4-dione

생성물 1

HCID 30590036-Hydroxy-8-methyl-3-(2-methylpropyl)-3,9-dihydro-2H-purin-2-one

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

10 g of 5,6-diamino-1-(2-methylpropyl)-2,4-(1H,3H)-pyrimidine dione was refluxed in 50 ml of acetic acid for 1 hour. 30 ml of chloroform was added and ether was then added slowly. The received crystals were filtered off. Yield 10.8 g. The amide was refluxed in 30 ml of 2N NaOH for 1 hour and then neutralized with 5N HCl. The crystals were filtered off and recrystallized from 50 ml of acetic acid. Yield 3.3 g. NMR (see Table I).

후처리

  1. filtrationThe received crystals were filtered off
  2. temperatureThe amide was refluxed in 30 ml of 2N NaOH for 1 hour
  3. filtrationThe crystals were filtered off
  4. customrecrystallized from 50 ml of acetic acid

출처 및 근거

ORD 기록
ord-5b8ad565345e41798ec6deb220cdcd93
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04644001

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