Theophylline → Diethyl [4-(1,3-dimethylxanthin-7-yl)butyl]phosphonate

HRID 1985

반응식

HRID 1985 반응식
[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[NH:9][CH:8]=[N:7][C:6]=2[N:5]([CH3:13])[C:3]1=[O:4].Cl[CH2:15][CH2:16][CH2:17][CH2:18][P:19]([O:24][CH2:25][CH3:26])(=[O:23])[O:20][CH2:21][CH3:22].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[N:9]([CH2:15][CH2:16][CH2:17][CH2:18][P:19](=[O:23])([O:24][CH2:25][CH3:26])[O:20][CH2:21][CH3:22])[CH:8]=[N:7][C:6]=2[N:5]([CH3:13])[C:3]1=[O:4]

참가 물질

5

반응물 3

HCID 2153TheophyllineHCID 11430Potassium CarbonateHCID 19689195Diethyl(4-chlorobutyl)phosphonate

생성물 1

HCID 22446301Diethyl [4-(1,3-dimethylxanthin-7-yl)butyl]phosphonate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

10.9 g (0.05 mol) of 1,3-dimethylxanthine were suspended in 150 ml of DMF, treated with 13.7 g (0.06 mol) of diethyl 4-chlorobutanephosphonate and 7.0 g (0.05 mol) of activated potassium carbonate and heated at 70° C. for approximately 4 hours. The solid was then filtered off, the filtrate was concentrated under reduced pressure and the oily residue which remained was taken up in ethyl acetate, filtered again and crystallized from diisopropyl ether.

후처리

  1. filtrationThe solid was then filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. filtrationfiltered again
  4. customcrystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-126b62e8f9c14b19bd96ee46b744d0b7
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728686

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