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

HRID 1588731노트

반응식

HRID 1588731 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4e2d530742674a908b1adf5ecaaab02d
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05223513

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