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

HRID 1421231
ノート
印刷プレビュー

反応式

HRID 1421231 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 147126087-Benzyl-3,8-dimethylxanthine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-abed677c7c934476abfd167829b6f730
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06075029

反応ノート

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