Dimethylformamide → HCID 18332796, 화합물

HRID 2269082노트

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HRID 2269082 반응식
CN(C=O)C.[H-].[Na+].[CH3:8][CH:9]([CH2:12][CH3:13])[CH2:10][SH:11].[NH2:14][C:15]1[N:23]=[C:22](Cl)[N:21]=[C:20]2[C:16]=1[N:17]=[CH:18][N:19]2[CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>[Cl-].[Na+].O>[NH2:14][C:15]1[N:23]=[C:22]([S:11][CH2:10][CH:9]([CH3:8])[CH2:12][CH3:13])[N:21]=[C:20]2[C:16]=1[N:17]=[CH:18][N:19]2[CH2:25][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 158772-Methyl-1-butanethiolHCID 24758Sodium hydrideHCID 2764829-Benzyl-2-chloro-9h-purin-6-amine

생성물 1

HCID 18332796HCID 18332796, 화합물수율 32%

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

반응 조건

온도
100 °C

실험 절차

To DMF suspension (10 ml) containing sodium hydride (300 mg, 7.5 mmol, 60% in mineral oil) were added 2-methylbutane-1-thiol (1 ml, 8.0 mmol) and 6-amino-9-benzyl-2-chloropurine (200 mg, 0.77 mmol) in order. The mixture was stirred under heating at 100° C. for 4.5 hours. Brine was added thereto and the mixture was extracted with chloroform. The organic layer was dried on magnesium sulfate, filtered and the solvent in the filtrate was evaporated in vacuo. The residue was purified with silica gel chromatography (1% methanol/chloroform) to give the subject compound (80 mg, yield 32%).

후처리

  1. extractionthe mixture was extracted with chloroform
  2. customThe organic layer was dried on magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent in the filtrate was evaporated in vacuo
  5. customThe residue was purified with silica gel chromatography (1% methanol/chloroform)

출처 및 근거

ORD 기록
ord-48c332c2faca471788bebf4901370240
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329381B1

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