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Benzyl Bromide → 7-Benzyl-3,8-dimethylxanthine

HRID 1421231
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HRID 1421231 반응식
[OH-].[Na+].[CH3:3][N:4]1[C:12]2[N:11]=[C:10]([CH3:13])[NH:9][C:8]=2[C:7](=[O:14])[NH:6][C:5]1=[O:15].[CH2:16](Br)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O.CO>[CH2:16]([N:9]1[C:8]2[C:7](=[O:14])[NH:6][C:5](=[O:15])[N:4]([CH3:3])[C:12]=2[N:11]=[C:10]1[CH3:13])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7498Benzyl BromideHCID 14798Sodium HydroxideHCID 179959183,8-Dimethyl-3,7-dihydro-1H-purine-2,6-dione

생성물 1

HCID 147126087-Benzyl-3,8-dimethylxanthine

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A solution of sodium hydroxide (400 mg) in water (5 ml) was added to a suspension of 3,8-dimethylxanthine (1.80 g) in methanol (10 ml) at 70° C. and stirred for 1 hour. Benzyl bromide (1.2 ml) was added and the mixture was stirred at 70-80° C. for 5 hours. After evaporation of the solvent under reduced pressure, the residue was suspended in saturated aqueous ammonium chloride solution (50 ml) and extracted with ethyl acetate (3×75 ml). The combined extracts were washed with saturated aqueous sodium chloride solution (30 ml), dried over magnesium sulfate and concentrate. The product was purified by recrystallization from ethanol. Yield=1.06 g.

후처리

  1. stirringthe mixture was stirred at 70-80° C. for 5 hours
  2. customAfter evaporation of the solvent under reduced pressure
  3. extractionextracted with ethyl acetate (3×75 ml)
  4. washThe combined extracts were washed with saturated aqueous sodium chloride solution (30 ml)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrate
  7. customThe product was purified by recrystallization from ethanol

출처 및 근거

ORD 기록
ord-abed677c7c934476abfd167829b6f730
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06075029

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