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

HRID 1291377ノート

反応式

HRID 1291377 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-119c7775fccb4d41a18c5e0954021bcf
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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