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

HRID 2296423

反応式

HRID 2296423 の反応式
[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

参加物

6

反応物 4

HCID 7616TripropylamineHCID 11788GlycosmicineHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 86738818Tri-n-propylamine chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-17061e7924be45d094b08c59460e6e0b
出典データセット
uspto-grants-1984_01
特許番号
US04429126

関連ノート

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