Allyl bromide → 7-Allyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione

HRID 1791998

反応式

HRID 1791998 の反応式
[Cl:1][C:2]1[NH:10][C:9]2[C:8](=[O:11])[N:7]([CH3:12])[C:6](=[O:13])[N:5]([CH3:14])[C:4]=2[N:3]=1.[CH2:15](Br)[CH:16]=[CH2:17].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:17]([N:10]1[C:9]2[C:8](=[O:11])[N:7]([CH3:12])[C:6](=[O:13])[N:5]([CH3:14])[C:4]=2[N:3]=[C:2]1[Cl:1])[CH:16]=[CH2:15]

参加物

5

反応物 3

HCID 7841Allyl bromideHCID 106618-ChlorotheophyllineHCID 11430Potassium Carbonate

生成物 1

HCID 7386827-Allyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (10.7 g), allyl bromide (5.2 ml), anhydrous potassium carbonate (10.3 g), and N,N-dimethylformamide (75 ml) was stirred at room temperature overnight. The reaction mixture was extracted with ethyl acetate and water, and the organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and filtered through a small amount of silica gel. The silica gel was washed with ethyl acetate, and the eluate was concentrated under reduced pressure. Recrystallization of the residue from ethyl acetate (50 ml) and hexane (100 ml) gave 10.57 g of the title compound.

後処理

  1. extractionThe reaction mixture was extracted with ethyl acetate and water
  2. washthe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered through a small amount of silica gel
  5. washThe silica gel was washed with ethyl acetate
  6. concentrationthe eluate was concentrated under reduced pressure
  7. customRecrystallization of the residue from ethyl acetate (50 ml) and hexane (100 ml)

出典と根拠

ORDレコード
ord-8be18deaea584ea4b6ab79b4a47d0b61
出典データセット
uspto-grants-2006_07
特許番号
US07074798B2

関連ノート

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