Phosphorus oxychloride → 2-Chloro-6,7-dihydro-9,10-dimethoxy-4H-pyrimido[6,1-a]isoquinolin-4-one

HRID 435156ノート

反応式

HRID 435156 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][N:13]2[C:20](=O)[CH2:19][C:17](=O)[NH:16][C:14]2=[O:15])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].P(Cl)(Cl)([Cl:24])=O>>[Cl:24][C:17]1[CH:19]=[C:20]2[C:6]3[C:5]([CH2:11][CH2:12][N:13]2[C:14](=[O:15])[N:16]=1)=[CH:4][C:3]([O:2][CH3:1])=[C:8]([O:9][CH3:10])[CH:7]=3

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 31526701-[2-(3,4-Dimethoxy-phenyl)-ethyl]-pyrimidine-2,4,6-trione

生成物 1

HCID 46787202-Chloro-6,7-dihydro-9,10-dimethoxy-4H-pyrimido[6,1-a]isoquinolin-4-one

実験手順

A mixture of 1-(3,4-dimethoxyphenylethyl)barbituric acid (20.2 g) and phosphorus oxychloride (100 ml) is refluxed for 2.5 hours at 100°-110° C. The excess of phosphorus oxychloride is distilled. The residue is poured onto crushed ice and made basic with a cold solution of 30% aqueous sodium hydroxide. A yellow gummy precipitate is separated and extracted with chloroform. The extract is washed with water, dried over sodium sulfate and concentrated to dryness under reduced pressure. The residue is purified by passage over a silica gel column using chloroform as eluent to give the desired compound.

後処理

  1. temperatureis refluxed for 2.5 hours at 100°-110° C
  2. distillationThe excess of phosphorus oxychloride is distilled
  3. additionThe residue is poured
  4. customonto crushed ice
  5. customA yellow gummy precipitate is separated
  6. extractionextracted with chloroform
  7. washThe extract is washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated to dryness under reduced pressure
  10. customThe residue is purified by passage over a silica gel column

出典と根拠

ORDレコード
ord-23566a1230e144ce805ae36dd1db962d
出典データセット
uspto-grants-1983_08
特許番号
US04400506

反応ノート

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