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

HRID 1985

反応式

HRID 1985 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-126b62e8f9c14b19bd96ee46b744d0b7
出典データセット
uspto-grants-1998_03
特許番号
US05728686

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