Phosphorus oxychloride → 4-Chloro-2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydroquinazoline

HRID 1354096ノート

反応式

HRID 1354096 の反応式
[CH3:1][C:2]1[N:11]=[C:10](O)[C:9]2[CH2:8][CH2:7][CH2:6][C:5]([CH3:19])([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:4]=2[N:3]=1.P(Cl)(Cl)([Cl:22])=O>>[Cl:22][C:10]1[C:9]2[CH2:8][CH2:7][CH2:6][C:5]([CH3:19])([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:4]=2[N:3]=[C:2]([CH3:1])[N:11]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178433414HCID 178433414、化合物

生成物 1

HCID 211043804-Chloro-2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydroquinazoline

実験手順

A mixture of 2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydro-quinazolin-4-ol (4 g, 16 mmol) and 25 mL of phosphorous oxychloride was heated under reflux for 2 hours, concentrated under reduced pressure and ice, water and dichloromethane were added. The mixture was basified with aqueous sodium carbonate and the organic layer was dried (sodium sulfate) and evaporated to afford 4.4 g of 4-chloro-2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydroquinazoline as an oil.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. concentrationconcentrated under reduced pressure and ice, water and dichloromethane
  4. additionwere added
  5. dry with materialthe organic layer was dried (sodium sulfate)
  6. customevaporated

出典と根拠

ORDレコード
ord-b398dc5a99ab4f8e82ea04d69a9a9470
出典データセット
uspto-grants-2007_05
特許番号
US07223767B2

反応ノート

読み込み中…