Potassium Carbonate → 1-(6-Oxoheptyl)-3-methyl-7-propylxanthine

HRID 582238노트

반응식

HRID 582238 반응식
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][CH2:12][CH3:13])[C:6]=2[C:5](=[O:14])[NH:4][C:3]1=[O:15].Cl[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][C:22](=[O:24])[CH3:23].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[O:24]=[C:22]([CH3:23])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][N:4]1[C:5](=[O:14])[C:6]2[N:7]([CH2:11][CH2:12][CH3:13])[CH:8]=[N:9][C:10]=2[N:2]([CH3:1])[C:3]1=[O:15]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 33143973-Methyl-7-propylpurine-2,6-dioneHCID 108445411-Chloro-heptan-6-one

생성물 1

HCID 218393431-(6-Oxoheptyl)-3-methyl-7-propylxanthine수율 162.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.1 g of 3-methyl-7-propylxanthine, 0.7 g of 1-chloro-heptan-6-one and 1.4 g of potassium carbonate are heated at 120° C. in 15 ml of dimethylformamide for 7.5 hours, while stirring. After the mixture has been concentrated under reduced pressure, the residue is poured into 100 ml of H2O, the mixture is extracted three times with 100 ml of CHCl3 each time, and the combined chloroform extracts are treated with 1 N sodium hydroxide solution and water in succession and dried over sodium sulfate. The concentration residue is chromatographed in a column using silica gel 60 and chloroform/ethanol (9:1) as the mobile phase. After recrystallization from petroleum ether/diisopropyl ether (3:1), 2.45 g (=76.6% yield) of 1-(6-oxoheptyl)-3-methyl-7-propylxanthine of melting point 69-70° C. are obtained.

후처리

  1. concentrationAfter the mixture has been concentrated under reduced pressure
  2. additionthe residue is poured into 100 ml of H2O
  3. extractionthe mixture is extracted three times with 100 ml of CHCl3 each time
  4. additionthe combined chloroform extracts are treated with 1 N sodium hydroxide solution and water in succession
  5. dry with materialdried over sodium sulfate
  6. customThe concentration residue is chromatographed in a column

출처 및 근거

ORD 기록
ord-e694167c4e8c41c3bc5e3de0e485612d
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922868

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