Reaktion #360977

Reaktionsgleichung

2-chloromethyl-6-methyl-3H-quina-zolin-4-one

phosphorus oxychloride

→

4-chloro-2-(chloromethyl)-6-methylquinazoline

Lösungsmittel

chloroform

N,N,4-trimethylaniline

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturat reflux temperature for 20 h
3. 3
   SonstigeThe reaction mixture is evaporated in a vacuum
4. 4
   workup.DISSOLUTIONThe residue is dissolved in 1.0 l of ethyl acetate
5. 5
   Waschenwashed in succession with 2N hydrochloric acid, water, saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution
6. 6
   EinengenThe organic extracts are concentrated to about 0.51 in a vacuum
7. 7
   workup.WAITThe mixture is left
8. 8
   Sonstigeto crystallize at -25° C. overnight
9. 9
   FiltrationThe crystal slurry is filtered
10. 10
    Waschenthe crystals are washed with ethyl acetate (-25° C.)
11. 11
    Sonstigedried in a vacuum

Vorschrift

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.

Quelle