Bromine → 2,6-Diamino-9-benzyl-8-bromopurine

HRID 2269123

반응식

HRID 2269123 반응식
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:4]([NH2:18])[N:3]=1.[Br:19]Br.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(Cl)Cl>[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[C:7]([Br:19])[N:8]2[CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:4]([NH2:18])[N:3]=1

참가 물질

5

반응물 3

HCID 24408BromineHCID 24477Sodium ThiosulfateHCID 2389302,6-Diamino-9-benzylpurine

생성물 1

HCID 183327282,6-Diamino-9-benzyl-8-bromopurine수율 47%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2,6-Diamino-9-benzylpurine (1.00 g, 4.16 mmol) and bromine (1 ml) were dissolved in 100 ml of methylene chloride and the solution was stirred at room temperature for 5 hours. Aqueous sodium thiosulfate was added to the reaction mixture. The organic layer was separated, dried on sodium sulfate and filtered. 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 (0.62 g, yield 47%).

후처리

  1. customThe organic layer was separated
  2. customdried on sodium 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-3fac389c22814ac58bf04c7647325a06
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329381B1

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