Enprofylline → 8-Chloro-3-propyl-3,7-dihydro-1H-purine-2,6-dione

HRID 2234924노트

반응식

HRID 2234924 반응식
[CH2:1]([N:4]1[C:12]2[N:11]=[CH:10][NH:9][C:8]=2[C:7](=[O:13])[NH:6][C:5]1=[O:14])[CH2:2][CH3:3].[Cl:15]N1C(=O)CCC1=O>CN(C=O)C>[Cl:15][C:10]1[NH:9][C:8]2[C:7](=[O:13])[NH:6][C:5](=[O:14])[N:4]([CH2:1][CH2:2][CH3:3])[C:12]=2[N:11]=1

참가 물질

4

반응물 2

HCID 1676EnprofyllineHCID 31398Chlorosuccinimide

생성물 1

HCID 113452208-Chloro-3-propyl-3,7-dihydro-1H-purine-2,6-dione수율 43.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-Propyl-3,7-dihydro-1H-purine-2,6-dione (J.Med.Chem, 1993, 36 (10), 1380-6) (0.3 g, 1.5 mmol) and N-chlorosuccinimide (0.21 g, 1.5 mmol) were dissolved in DMF (5 ml) and the solution stirred for 5 h. The solution was concentrated and the solid residues washed with methanol and filtered to provide the product as a white solid (0.148 g, 42%). NMR; δH (400 MHz, d6-DMSO) 0.85 (t, 3H, J=7 Hz), 1.65 (m, 2H), 3.8 (t, 2H, J=7 Hz), 11.2 (s, 1H), one exchangeable not observed to δH 13; m/z 229[MH+]

후처리

  1. concentrationThe solution was concentrated
  2. washthe solid residues washed with methanol
  3. filtrationfiltered

출처 및 근거

ORD 기록
ord-49e759ccba6b442488eeb8976a1a1529
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713982B2

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