Phosphorus oxychloride → HCID 20093927、化合物

HRID 273795

反応式

HRID 273795 の反応式
[Cl:1][CH2:2][C:3]1[NH:12][C:11](=O)[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([CH3:14])[CH:9]=2)[N:4]=1.P(Cl)(Cl)([Cl:17])=O>C(Cl)(Cl)Cl.CN(C)C1C=CC(C)=CC=1>[Cl:17][C:11]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([CH3:14])[CH:9]=2)[N:4]=[C:3]([CH2:2][Cl:1])[N:12]=1

参加物

5

反応物 2

HCID 24813Phosphorus oxychlorideHCID 1357150192-(chloromethyl)-6-methylquinazolin-4(3H)-one

生成物 1

HCID 20093927HCID 20093927、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 7471Dimethyl-p-toluidine溶媒

実験手順

2. 114.1 g of 2-chloromethyl-6-methyl-3H-quina-zolin-4-one are dissolved in 1.11 of chloroform and 120 ml of N,N,4-trimethylaniline, treated with 53 ml of phosphorus oxychloride and heated at reflux temperature for 20 h. The reaction mixture is evaporated in a vacuum. The residue is dissolved in 1.0 l of ethyl acetate and washed in succession with 2N hydrochloric acid, water, saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution. The organic extracts are concentrated to about 0.51 in a vacuum. The mixture is left to crystallize at -25° C. overnight. The crystal slurry is filtered, the crystals are washed with ethyl acetate (-25° C.) and dried in a vacuum. 89.9 g of 4-chloro-2-(chloromethyl)-6-methylquinazoline of m.p. 111°-112° C. are obtained. A further 11.1 g of 4-chloro-2-(chloromethyl)-6-methylquinazoline of m.p. 114°-116° C. can be obtained from the mother liquor.

後処理

  1. temperatureheated
  2. temperatureat reflux temperature for 20 h
  3. customThe reaction mixture is evaporated in a vacuum
  4. dissolutionThe residue is dissolved in 1.0 l of ethyl acetate
  5. washwashed in succession with 2N hydrochloric acid, water, saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution
  6. concentrationThe organic extracts are concentrated to about 0.51 in a vacuum
  7. waitThe mixture is left
  8. customto crystallize at -25° C. overnight
  9. filtrationThe crystal slurry is filtered
  10. washthe crystals are washed with ethyl acetate (-25° C.)
  11. customdried in a vacuum

出典と根拠

ORDレコード
ord-ec8e685dcf3944b5b17a6d6282cdecb5
出典データセット
uspto-grants-1995_02
特許番号
US05387585

関連ノート

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