Ethyl orthoformate → HCID 11777595, 화합물

HRID 883548노트

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HRID 883548 반응식
[NH2:1][C:2]1[C:3](=[O:17])[NH:4][C:5](=[S:16])[N:6]([CH2:9][CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[C:7]=1[NH2:8].[CH:18](OCC)(OCC)OCC>CCCCCCC>[CH:10]1([CH2:9][N:6]2[C:7]3[N:8]=[CH:18][NH:1][C:2]=3[C:3](=[O:17])[NH:4][C:5]2=[S:16])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1

참가 물질

4

반응물 2

HCID 31214Ethyl orthoformateHCID 86601053HCID 86601053, 화합물

생성물 1

HCID 11777595HCID 11777595, 화합물수율 63%

시약·촉매·용매 1

HCID 8900Heptane용매

실험 절차

5,6-Diamino-1-cyclohexylmethyl-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one, (1.44 g, 5.67 mmol) together with triethyl orthoformate (15 mL) was heated at 146° C. for 2 h and 10 minutes. The mixture was allowed to cool to ambient temperature and then further cooled on an ice-bath, followed by addition of heptane (5 mL). After filtration of the suspension and washing with heptane (20 mL), the obtained solid was dried in vacuo. Suspending the solid (1.2 g) in a hot mixture of 2-propanol (125 mL), water (5 mL) and tert-butyl methyl ether (25 mL) gave, after cooling and filtration, a white precipitate which was washed with further tert-butyl methyl ether (5 mL). The solid was dried in vacuo to give the title compound (0.95 g, 63%).

후처리

  1. temperaturefurther cooled on an ice-bath
  2. filtrationAfter filtration of the suspension
  3. washwashing with heptane (20 mL)
  4. customthe obtained solid was dried in vacuo
  5. additionin a hot mixture of 2-propanol (125 mL), water (5 mL) and tert-butyl methyl ether (25 mL)
  6. customgave
  7. temperatureafter cooling
  8. filtrationfiltration
  9. washa white precipitate which was washed with further tert-butyl methyl ether (5 mL)
  10. customThe solid was dried in vacuo

출처 및 근거

ORD 기록
ord-f480426822fc4452beda613e0abf40ab
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08236951B2

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