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Potassium Carbonate → HCID 22007313, 화합물

HRID 323870
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HRID 323870 반응식
C(=O)([O-])[O-].[K+].[K+].[CH2:7]([N:14]1[C:22]2[C:21](=[O:23])[NH:20][C:19](=[O:24])[N:18]([CH2:25][CH3:26])[C:17]=2[N:16]=[CH:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH:27]([O:31][CH2:32]Cl)([CH2:29][CH3:30])[CH3:28]>CN(C)C=O.O.CO>[CH2:7]([N:14]1[C:22]2[C:21](=[O:23])[N:20]([CH2:32][O:31][CH:27]([CH2:29][CH3:30])[CH3:28])[C:19](=[O:24])[N:18]([CH2:25][CH3:26])[C:17]=2[N:16]=[CH:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
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참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 13089848HCID 13089848, 화합물2회HCID 220073037-Benzyl-3-ethyl-3,7-dihydro-1H-purine-2,6-dione

생성물 1

HCID 22007313HCID 22007313, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매2회
HCID 6228
Dimethylformamide
용매

실험 절차

2.45 g (18.0 mmol) of potassium carbonate were added at 60° C. to a suspension of 3.0 g (11.0 mmol) of 7-benzyl-3-ethylxanthine (prepared according to Example 5a) in 60 ml of dimethylformamide and the mixture was stirred at this temperature for one hour. 1.77 g (14.0 mmol) of sec-butoxymethyl chloride were then added dropwise and the mixture was stirred at 80° C. for 5 hours. 0.7 g (5.5 mmol) of sec-butoxymethyl chloride was then added again and the mixture was stirred for a further 3 hours. 12 ml of water and 5 ml of methanol were then added and the mixture was stirred at 50° C. for 2 hours. A further 60 ml of water were then added, the mixture was extracted three times using 200 ml of methyl tert-butyl ether each time, and the combined organic phases were washed with 200 ml of water, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, dichloromethane/methanol (19.8/0.2).

후처리

  1. stirringthe mixture was stirred at 80° C. for 5 hours
  2. stirringthe mixture was stirred for a further 3 hours
  3. stirringthe mixture was stirred at 50° C. for 2 hours
  4. extractionthe mixture was extracted three times
  5. washthe combined organic phases were washed with 200 ml of water
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customThe crude product was purified by flash chromatography on a silica gel column, dichloromethane/methanol (19.8/0.2)

출처 및 근거

ORD 기록
ord-1da0011b7c894f59954ed41089530c74
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06214992B1

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