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

HRID 2016

反応式

HRID 2016 の反応式
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[NH:14][C:13](=[O:18])[N:12]([CH3:19])[C:11]=2[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:21][CH2:22][CH2:23][CH2:24][P:25]([O:30][CH2:31][CH3:32])(=[O:29])[O:26][CH2:27][CH3:28].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:21][CH2:22][CH2:23][CH2:24][P:25](=[O:29])([O:30][CH2:31][CH3:32])[O:26][CH2:27][CH3:28])[C:13](=[O:18])[N:12]([CH3:19])[C:11]=2[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 6856307-Benzyl-3-methylxanthineHCID 19689195Diethyl(4-chlorobutyl)phosphonate

生成物 1

HCID 22446297Diethyl [4-(7-benzyl-3-methylxanthin-1-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

20.4 g (0.08 mol) of 7-benzyl-3-methylxanthine were suspended in 200 ml of dimethylformamide (DMF), treated with 22 g (0.96 mol) of diethyl 4-chlorobutanephosphonate and 13.8 g (0.1 mol) of activated potassium carbonate and heated at 70° C. for 4 hours and filtered, 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. filtrationfiltered
  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-7a6debe642dd4a55a17f79ac83e9ef86
出典データセット
uspto-grants-1998_03
特許番号
US05728686

関連ノート

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