Iodoethane → Diethyl [4-(7-ethyl-3-methylxanthin-1-yl)butyl]phosphonate

HRID 2023

反応式

HRID 2023 の反応式
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][NH:7][C:6]=2[C:5](=[O:11])[N:4]([CH2:12][CH2:13][CH2:14][CH2:15][P:16](=[O:23])([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[C:3]1=[O:24].[CH2:25](I)[CH3:26].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:25]([N:7]1[C:6]2[C:5](=[O:11])[N:4]([CH2:12][CH2:13][CH2:14][CH2:15][P:16](=[O:23])([O:17][CH2:18][CH3:19])[O:20][CH2:21][CH3:22])[C:3](=[O:24])[N:2]([CH3:1])[C:10]=2[N:9]=[CH:8]1)[CH3:26]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 22446315Diethyl [4-(3-methylxanthin-1-yl)butyl]phosphonate

生成物 1

HCID 22446294Diethyl [4-(7-ethyl-3-methylxanthin-1-yl)butyl]phosphonate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

7.2 g (0.02 mol) of diethyl [4-(3-methylxanthin-1-yl)-butyl]phosphonate were suspended in 100 ml of DMF, treated with 4.7 g (0.03 mol) of ethyl iodide and 4.1 g (0.03 mol) of activated potassium carbonate and heated at 60° C. for 4 hours. The solid was 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 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-056956b73b9f45e9955998f708e34b9b
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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