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

HRID 376243

반응식

HRID 376243 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH:6]=[CH2:7].[H-].[Na+].[CH3:10][N:11]1[C:19]2[N:18]=[CH:17][N:16]([CH3:20])[C:15]=2[C:14](=[O:21])[NH:13][C:12]1=[O:22].O>CS(C)=O>[CH2:2]([N:13]1[C:14](=[O:21])[C:15]2[N:16]([CH3:20])[CH:17]=[N:18][C:19]=2[N:11]([CH3:10])[C:12]1=[O:22])[CH2:3][CH2:4][CH2:5][CH:6]=[CH2:7]

참가 물질

6

반응물 4

HCID 962WaterHCID 5429TheobromineHCID 24758Sodium hydrideHCID 759066-Bromo-1-hexene

생성물 1

HCID 128776801-(Hex-5-en-1-yl)-3,7-dimethyl-3,7-dihydro-1H-purine-2,6-dione수율 98.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

1-(5,6-Oxidohexyl)-3,7-dimethylxanthine was synthesized and used as an intermediate for synthesizing inventive compounds nos. 1517 and 1595 as described in examples 2 and 3 below. A mixture of l-bromo-5-hexene (10.7 g, 66 mmol), sodium hydride (1.58 g, 66 mmol), and 3,7-dimethylxanthine (11.9 g, 66 mmol) in dimethylsulfoxide (100 ml) was stirred for 43 hr. The solution was treated with water (200 ml) and then extracted with dichloromethane (3×80 ml). The combined extracts were washed with water (3×100 ml), dried over magnesium sulfate, and then the solvent was evaporated under vacuum to give 1-(5-hexenyl)-3,7-dimethylxanthine (17 g, 98% yield) as a white powder.

후처리

  1. customused as an intermediate for synthesizing inventive compounds nos
  2. extractionextracted with dichloromethane (3×80 ml)
  3. washThe combined extracts were washed with water (3×100 ml)
  4. dry with materialdried over magnesium sulfate
  5. customthe solvent was evaporated under vacuum

출처 및 근거

ORD 기록
ord-0932809fb3584dd78277345915f73256
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06020337

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