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Thionyl Chloride → 4-Chloro-6-methyl-2-phenylquinazoline

HRID 1973871
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반응식

HRID 1973871 반응식
[CH3:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[NH:6][C:5]2=O.S(Cl)([Cl:21])=O>CN(C)C=O>[Cl:21][C:5]1[C:4]2[C:9](=[CH:10][CH:11]=[C:2]([CH3:1])[CH:3]=2)[N:8]=[C:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 1356776016-Methyl-2-phenyl-4(3H)-quinazolinone

생성물 1

HCID 214906444-Chloro-6-methyl-2-phenylquinazoline

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred slurry of 2.1 g of 6-methyl-2-phenylquinazolin-4(3H)-one and 35 ml of thionyl chloride was added dropwise 1.3 g of dimethylformamide. The mixture was maintained at reflux temperature for 90 minutes. The mixture was concentrated under reduced pressure, the residual solid was mixed with crushed ice and the washed solid collected. Two recrystallizations from petroleum ether (60°-110° fraction) gave 1.5 g of 4-chloro-6-methyl-2-phenylquinazoline, m.p. 111°-113°.

후처리

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  1. temperatureThe mixture was maintained
  2. temperatureat reflux temperature for 90 minutes
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additionthe residual solid was mixed with crushed ice
  5. customthe washed solid collected
  6. customTwo recrystallizations from petroleum ether (60°-110° fraction)

출처 및 근거

ORD 기록
ord-a8209c96ebd442b0b2a9268207697c9f
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03998951

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