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

HRID 2269123

反応式

HRID 2269123 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 183327282,6-Diamino-9-benzyl-8-bromopurine収率 47%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-3fac389c22814ac58bf04c7647325a06
出典データセット
uspto-grants-2001_12
特許番号
US06329381B1

関連ノート

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