Methyl iodide → 8-Bromo-3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione

HRID 1835727

반응식

HRID 1835727 반응식
[Br:1][C:2]1[NH:10][C:9]2[C:8](=[O:11])[NH:7][C:6](=[O:12])[N:5]([CH3:13])[C:4]=2[N:3]=1.[C:14](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O>[Br:1][C:2]1[N:10]([CH3:14])[C:9]2[C:8](=[O:11])[NH:7][C:6](=[O:12])[N:5]([CH3:13])[C:4]=2[N:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 15487978-bromo-3-methyl-3,7-dihydro-1H-purine-2,6-dione

생성물 1

HCID 7022428-Bromo-3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione수율 93.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirring suspension of 8-bromo-3-methylxanthine (prepared as described above for CT12440) (12.25 g, 50.0 mmol) and potassium carbonate (8.62 g, 62.5 mmol) in dimethylformamide (150 ml) was added methyl iodide (7.81 g, 55.0 mmol). After stirring overnight at room temperature, the mixture was poured into ice cold water (400 ml) and stirred at 0-5° C. for 1 hour. The precipitate was filtered, rinsed with water (5×25 ml) and dried under vacuum to provide 8-bromo-3,7-dimethylxanthine (12.10 g, 93% yield) as a beige solid.

후처리

  1. stirringstirred at 0-5° C. for 1 hour
  2. filtrationThe precipitate was filtered
  3. washrinsed with water (5×25 ml)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-b10c9ede3c1345008b12f267197c0d9e
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06774130B2

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