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

HRID 1791998노트

반응식

HRID 1791998 반응식
[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]

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 106618-ChlorotheophyllineHCID 11430Potassium Carbonate

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8be18deaea584ea4b6ab79b4a47d0b61
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07074798B2

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