Tripropylamine → 4-Chloro-1-methylquinazolin-2(1H)-one

HRID 2296423

반응식

HRID 2296423 반응식
[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5](=O)[NH:4][C:3]1=[O:13].C(N(CCC)CCC)CC.P(Cl)(Cl)([Cl:26])=O.[OH-].[Na+]>C(N(CCC)CCC)CC.C(Cl)(Cl)Cl>[Cl:26][C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[N:2]([CH3:1])[C:3](=[O:13])[N:4]=1

참가 물질

6

반응물 4

HCID 7616TripropylamineHCID 11788GlycosmicineHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychloride

생성물 1

HCID 134883764-Chloro-1-methylquinazolin-2(1H)-one

시약·촉매·용매 1

HCID 86738818Tri-n-propylamine chloroform용매

실험 절차

A mixture of 1-methylquinazoline-2,4-dione (8.8 g), tri-n-propylamine (8.6 g) and phosphorus oxychloride (80 ml) was stirred for 1 hour at 110°-120° C. The resultant mixture was cooled to ambient temperature and concentrated under reduced pressure to give a residue, which was dissolved in 2% tri-n-propylamine-chloroform solution. The solution was added dropwise to a mixture of 2 N sodium hydroxide aqueous solution and ice at alkaline pH. The aqueous layer was separated and extracted twice with chloroform. The combined chloroform layer was washed with water and with aqueous solution saturated with sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give crystalline 4-chloro-1-methyl-1H-quinazoline-2-one.

후처리

  1. concentrationconcentrated under reduced pressure
  2. customto give a residue, which
  3. customThe aqueous layer was separated
  4. extractionextracted twice with chloroform
  5. washThe combined chloroform layer was washed with water and with aqueous solution saturated with sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-17061e7924be45d094b08c59460e6e0b
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04429126

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