Potassium Carbonate → HCID 22007301, 화합물

HRID 323856

반응식

HRID 323856 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][CH2:26][CH3:27])[C:17]=2[N:16]=[CH:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH2:28]([O:30][CH2:31]Cl)[CH3:29]>CN(C)C=O.O.CO>[CH2:7]([N:14]1[C:22]2[C:21](=[O:23])[N:20]([CH2:31][O:30][CH2:28][CH3:29])[C:19](=[O:24])[N:18]([CH2:25][CH2:26][CH3:27])[C:17]=2[N:16]=[CH:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 18523Chloromethyl ethyl ether2회HCID 220073027-Benzyl-3-propylxanthine

생성물 1

HCID 22007301HCID 22007301, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매2회HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

1.71 g (12.0 mmol) of potassium carbonate were added to a hot solution of 2.2 g (7.7 mmol) of 7-benzyl-3-propylxanthine from stage a) in 60 ml of dimethylformamide at 60° C. and the mixture was stirred at 60° C. for 1 hour. 0.93 ml (10.0 mmol) of ethoxymethyl chloride was then added dropwise and the mixture was stirred at 80° C. for 4.5 hours. A further 0.5 ml (5.3 mmol) of ethoxymethyl chloride was then added and the mixture was again stirred for 6 hours. 12 ml of water and 5 ml of methanol were then added, the mixture was allowed to stand overnight, 60 ml of water were added again and the mixture was extracted three times using methyl tert-butyl ether. The combined organic phases were washed twice with 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 4.5 hours
  2. stirringthe mixture was again stirred for 6 hours
  3. waitto stand overnight
  4. extractionthe mixture was extracted three times
  5. washThe combined organic phases were washed twice with 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-fdfe6072ba324e2b8b4432b84f0efb8c
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06214992B1

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