Phosphorus oxychloride → HCID 20093927, 화합물

HRID 273795

반응식

HRID 273795 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 20093927HCID 20093927, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 7471Dimethyl-p-toluidine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ec8e685dcf3944b5b17a6d6282cdecb5
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387585

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