Potassium Carbonate → [1-(1,3-Dibutylxanthin-7-yl)methyl]dimethylphosphine Oxide

HRID 2050

反応式

HRID 2050 の反応式
[CH2:1]([N:5]1[C:14](=[O:15])[C:13]2[NH:12][CH:11]=[N:10][C:9]=2[N:8]([CH2:16][CH2:17][CH2:18][CH3:19])[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4].Cl[CH2:21][P:22](=[O:25])([CH3:24])[CH3:23].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:1]([N:5]1[C:14](=[O:15])[C:13]2[N:12]([CH2:21][P:22](=[O:25])([CH3:24])[CH3:23])[CH:11]=[N:10][C:9]=2[N:8]([CH2:16][CH2:17][CH2:18][CH3:19])[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 74224Phosphine oxide, (chloromethyl)dimethyl-HCID 1014211,3-Dibutylxanthine

生成物 1

HCID 19689263[1-(1,3-Dibutylxanthin-7-yl)methyl]dimethylphosphine Oxide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5 g (0.01 9 mol) of 1,3-dibutylxanthine were stirred at 80° C. for 6 hours with 2.88 g (0.0228 mol) of chloromethyldimethylphosphine oxide and 3.2 g (0.0228 mol) of potassium carbonate in 80 ml of DMF. The solution was cooled to room temperature and filtered, and the filtrate was concentrated under reduced pressure. The residue which remained was crystallized in petroleum ether/ethyl acetate.

後処理

  1. filtrationfiltered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue which remained was crystallized in petroleum ether/ethyl acetate

出典と根拠

ORDレコード
ord-20ece88fc4e64225b2c8a9f117afb490
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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