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

HRID 1354096노트

반응식

HRID 1354096 반응식
[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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178433414HCID 178433414, 화합물

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b398dc5a99ab4f8e82ea04d69a9a9470
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223767B2

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