Carbon Tetrachloride → 2-[4-[4-(2-Chloroethoxy)benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

HRID 1291377노트

반응식

HRID 1291377 반응식
[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[CH3:13])[N:4]=[C:3]1[S:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:33])[C:23]2[CH:28]=[CH:27][C:26]([O:29][CH2:30][CH2:31]O)=[CH:25][CH:24]=2)=[CH:18][CH:17]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:54]>>[Cl:54][CH2:31][CH2:30][O:29][C:26]1[CH:27]=[CH:28][C:23]([C:22]([C:19]2[CH:20]=[CH:21][C:16]([CH2:15][S:14][C:3]3[N:2]([CH3:1])[C:11](=[O:12])[C:10]4[C:5](=[CH:6][CH:7]=[CH:8][C:9]=4[CH3:13])[N:4]=3)=[CH:17][CH:18]=2)=[O:33])=[CH:24][CH:25]=1

참가 물질

4

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 189188073,5-dimethyl-2-[4-[4-(2-hydroxyethoxy)benzoyl]benzylthio]-4(3H)-quinazolinone

생성물 1

HCID 189188132-[4-[4-(2-Chloroethoxy)benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

실험 절차

To a suspension of 3,5-dimethyl-2-[4-[4-(2-hydroxyethoxy)benzoyl]benzylthio]-4(3H)-quinazolinone (651 mg) in carbon tetrachloride (15 ml) was added triphenylphosphine (476 mg) and the mixture was refluxed for 40 hours. This reaction mixture was concentrated and the residue was purified by silica gel column chromatography (dichloromethane) and recrystallized from ethyl acetate to provide the title compound as colorless solid (391 mg).

후처리

  1. temperaturethe mixture was refluxed for 40 hours
  2. concentrationThis reaction mixture was concentrated
  3. customthe residue was purified by silica gel column chromatography (dichloromethane)
  4. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-119c7775fccb4d41a18c5e0954021bcf
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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