Water → 1-(Hex-5-en-1-yl)-3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione

HRID 1870844

반응식

HRID 1870844 반응식
[NH:1]1[C:12](=[O:13])[C:11]2[N:9]([CH3:10])[CH:8]=[N:7][C:6]=2[N:4]([CH3:5])[C:2]1=[O:3].Br[CH:15]=[CH:16][CH2:17][CH2:18][CH2:19][CH3:20].[H-].[Na+].O>CS(C)=O>[CH2:20]([N:1]1[C:12](=[O:13])[C:11]2[N:9]([CH3:10])[CH:8]=[N:7][C:6]=2[N:4]([CH3:5])[C:2]1=[O:3])[CH2:19][CH2:18][CH2:17][CH:16]=[CH2:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 5429TheobromineHCID 24758Sodium hydrideHCID 2873381-Bromo-1-hexene

생성물 1

HCID 128776801-(Hex-5-en-1-yl)-3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione수율 98.5%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

Theobromine (11.9 g, 66 mmol, available from Sigma) was added to a mixture of bromohexene (10.7 g, 66 mmol, available from Aldrich) and sodium hydride (1.58 g, 66 mmol) in dimethylsulfoxide (100 ml) and the resulting mixture stirred for 43 hours. The solution was treated with water (200 ml) and then extracted with three 80 ml aliquots of dichloromethane. The combined extracts were washed with three 100 ml aliquots of water and dried over magnesium sulfate. The solvent was evaporated under vacuum, leaving 17 g of a white powder, 1-(5-hexenyl)-3,7-dimethylxanthine (65 mmol, 98% yield).

후처리

  1. extractionextracted with three 80 ml aliquots of dichloromethane
  2. washThe combined extracts were washed with three 100 ml aliquots of water
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated under vacuum

출처 및 근거

ORD 기록
ord-72e406083e07421382fc1fcb63a8f11b
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06100271

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