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

HRID 1814940

반응식

HRID 1814940 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 (5x 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 (5x 25 ml)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-9655b689d12b473bb284ec4c9816e161
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06878715B1

연결된 노트

불러오는 중…