Phosphorus oxychloride → 4-chloro-N,N-dimethylquinazolin-6-amine

HRID 596609노트

반응식

HRID 596609 반응식
[CH3:1][N:2]([CH3:14])[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][NH:7][C:6]2=O.P(Cl)(Cl)([Cl:17])=O>CCOCC>[CH3:1][N:2]([CH3:14])[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][N:7]=[C:6]2[Cl:17]

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 1358112116-(Dimethylamino)-3,4-dihydroquinazolin-4-one

생성물 1

HCID 233667574-chloro-N,N-dimethylquinazolin-6-amine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 12.4 g. of 6-dimethylamino-quinazolin-4(3H)-one and 50 ml. of phosphorus oxychloride is refluxed under nitrogen for 10 minutes, cooled to room temperature, 150 ml. of ether added, the crystals recovered by filtering, washed with ether and dried. The solids are added to 500 ml. of ice-water, concentrated ammonia is added to neutralize the solution which is extracted with 1.0 liter of chloroform. The chloroform extract is dried and filtered through 300 ml. of silica gel using chloroform as an eluant. Evaporation of the eluant yields 6-dimethylamino-4-chloroquinazoline, m.p. 126°-127.5° C.

후처리

  1. additionA mixture of 12.4 g
  2. customthe crystals recovered
  3. filtrationby filtering
  4. washwashed with ether
  5. customdried
  6. additionThe solids are added to 500 ml
  7. additionof ice-water, concentrated ammonia is added
  8. extractionis extracted with 1.0 liter of chloroform
  9. extractionThe chloroform extract
  10. customis dried
  11. filtrationfiltered through 300 ml
  12. customEvaporation of the eluant

출처 및 근거

ORD 기록
ord-4dc27b9c24534498909634ddcf26ab2e
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04011323

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