4-Chlorophenyl Isocyanate → N-(4-chlorophenyl)-N'-[4-(2-chlorophenyl)-1,2-dihydro-1,6,7-trimethyl-2-oxo-3-quinolyl]urea

HRID 1588731ノート

反応式

HRID 1588731 の反応式
[NH2:1][C:2]1[C:3](=[O:22])[N:4]([CH3:21])[C:5]2[C:10]([C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:18])=[CH:9][C:8]([CH3:19])=[C:7]([CH3:20])[CH:6]=2.[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([N:30]=[C:31]=[O:32])=[CH:26][CH:25]=1>C1C=CC=CC=1>[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([NH:30][C:31]([NH:1][C:2]2[C:3](=[O:22])[N:4]([CH3:21])[C:5]3[C:10]([C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])=[CH:9][C:8]([CH3:19])=[C:7]([CH3:20])[CH:6]=3)=[O:32])=[CH:26][CH:25]=1

参加物

4

反応物 2

HCID 76934-Chlorophenyl IsocyanateHCID 197544703-amino-4-(2-chlorophenyl)-1,6,7-trimethyl-2(1H)-quinolone

生成物 1

HCID 54113676N-(4-chlorophenyl)-N'-[4-(2-chlorophenyl)-1,2-dihydro-1,6,7-trimethyl-2-oxo-3-quinolyl]urea収率 80.8%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 3-amino-4-(2-chlorophenyl)-1,6,7-tri-methyl-2(1H)-quinolone (156 mg), 4-chlorophenyl isocyanate (115 mg) and benzene (4 ml) was refluxed for 1.5 hours and then distilled to remove the solvent. The remaining crystals as collected by filtration were washed with isopropyl ether to obtain N-(4-chlorophenyl)-N'-[4-(2-chlorophenyl) -1,2-dihydro-1,6,7-trimethyl-2-oxo-3-quinolyl]urea (188 mg, 80.7%). Recrystallization from acetone - hexane gave colorless needles. mp 207°-209° C.

後処理

  1. temperaturewas refluxed for 1.5 hours
  2. distillationdistilled
  3. customto remove the solvent
  4. filtrationThe remaining crystals as collected by filtration
  5. washwere washed with isopropyl ether

出典と根拠

ORDレコード
ord-4e2d530742674a908b1adf5ecaaab02d
出典データセット
uspto-grants-1993_06
特許番号
US05223513

反応ノート

読み込み中…