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Potassium Carbonate → Diethyl [4-(1-benzyl-3-methylxanthin-7-yl)butyl]phosphonate

HRID 1990
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HRID 1990 반응식
Cl.[CH2:2]([N:9]1[C:18](=[O:19])[C:17]2[NH:16][CH:15]=[N:14][C:13]=2[N:12]([CH3:20])[C:10]1=[O:11])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl[CH2:22][CH2:23][CH2:24][CH2:25][P:26]([O:31][CH2:32][CH3:33])(=[O:30])[O:27][CH2:28][CH3:29].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:2]([N:9]1[C:18](=[O:19])[C:17]2[N:16]([CH2:22][CH2:23][CH2:24][CH2:25][P:26](=[O:30])([O:31][CH2:32][CH3:33])[O:27][CH2:28][CH3:29])[CH:15]=[N:14][C:13]=2[N:12]([CH3:20])[C:10]1=[O:11])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 19689195Diethyl(4-chlorobutyl)phosphonateHCID 196892401-Benzyl-3-methylxanthine hydrochloride

생성물 1

HCID 22446290Diethyl [4-(1-benzyl-3-methylxanthin-7-yl)butyl]phosphonate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

20 g (0.078 mol) of 1-benzyl-3-methylxanthine hydrochloride, 21.4 g (0.094 mol) of diethyl 4-chlorobutanephosphonate and 26 g (0.2 mol) of potassium carbonate were suspended in 400 ml of dimethylformamide and stirred at 70° C. for 6 hours. The solution was filtered hot and the dimethylformamide was evaporated under reduced pressure. The oily residue which remained was taken up in dichloromethane and washed several times with water. After evaporating the solvent, it was possible to reuse the pale yellow, oily residue without purification.

후처리

  1. filtrationThe solution was filtered hot
  2. customthe dimethylformamide was evaporated under reduced pressure
  3. washwashed several times with water
  4. customAfter evaporating the solvent, it
  5. customwithout purification

출처 및 근거

ORD 기록
ord-1b88eb8cb6094a9a8d87846b4529cb21
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05728686

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