Phosphorus oxychloride → HCID 20093927, Verbindung

HRID 273795

Reaktionsgleichung

Reaktionsgleichung von HRID 273795
[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

Komponenten

5

Edukt 2

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

Produkt 1

HCID 20093927HCID 20093927, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 7471Dimethyl-p-toluidineLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-ec8e685dcf3944b5b17a6d6282cdecb5
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387585

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