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Potassium Carbonate → 8-Bromo-7-ethoxymethyl-3-methylxanthine

HRID 1814925
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반응식

HRID 1814925 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(=O)([O-])[O-].[K+].[K+].[CH2:20]([O:22][CH2:23]Cl)[CH3:21]>CN(C=O)C>[Br:1][C:2]1[N:10]([CH2:23][O:22][CH2:20][CH3:21])[C:9]2[C:8](=[O:11])[NH:7][C:6](=[O:12])[N:5]([CH3:13])[C:4]=2[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 18523Chloromethyl ethyl etherHCID 15487978-bromo-3-methyl-3,7-dihydro-1H-purine-2,6-dione

생성물 1

HCID 224991168-Bromo-7-ethoxymethyl-3-methylxanthine수율 70.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirring suspension of 8-bromo-3-methylxanthine (7.06 g, 28.8 mmol) and potassium carbonate (3.98 g, 28.8 mmol) in DMF (150 ml) was added chloromethyl ethyl ether (2.72 g, 28.8 mmol). After stirring overnight at room temperature, the reaction mixture was poured into ice-cold water (650 ml). After stirring at 0-5° C. for 1 hour, the cloudy mixture was filtered, washed with water (3x 15 ml) and dried under vacuum to provide 8-bromo-7-ethoxymethyl-3-methylxanthine (6.15 g, 70% yield) as a white solid.

후처리

  1. stirringAfter stirring at 0-5° C. for 1 hour
  2. filtrationthe cloudy mixture was filtered
  3. washwashed with water (3x 15 ml)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-65757a3858764547807de95017a19865
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06878715B1

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