Water → 1-(11-Dodecenyl)-3,7-dimethylxanthine

HRID 361531노트

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HRID 361531 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].[Na].CS([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH:29]=[CH2:30])(=O)=O.O>CS(C)=O>[CH2:30]([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])[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH:20]=[CH2:19]

참가 물질

5

반응물 3

HCID 962WaterHCID 2329589712-Methanesulfonyl-1-dodeceneHCID 66980828Theobromine sodium

생성물 1

HCID 232958711-(11-Dodecenyl)-3,7-dimethylxanthine수율 67%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
60 °C

실험 절차

To a suspension of sodium theobromine (6.00 g, 30.0 mmol) in dimethylsulfoxide (60 mL) was added 12-methanesulfonyl-1-dodecene and the reaction stirred for 16 hours at 60° C. The mixture was then poured into water (120 mL) and extracted with diethyl ether (2×100 mL). The organic portions were combined, dried using magnesium sulfate and evaporated to give a cream solid. Recrystallization from ethyl acetate/hexane 1:1 yields 6.97 g (67% yield) 1-(11-dodecenyl)-3,7-dimethylxanthine (inventive compound no. 2516) as a white solid.

후처리

  1. extractionextracted with diethyl ether (2×100 mL)
  2. customdried
  3. customevaporated
  4. customto give a cream solid
  5. customRecrystallization from ethyl acetate/hexane 1:1

출처 및 근거

ORD 기록
ord-3b99d46d7b2847a18e391c7e79ec13d2
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866576

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