2-Amino-4'-chlorobenzophenone → 6-(4-Chlorophenyl)-11H-pyrido[2,3-b][1,4]benzodiazepine

HRID 637456노트

반응식

HRID 637456 반응식
[NH2:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1)=O.[NH2:17][C:18]1[C:19](Cl)=[N:20][CH:21]=[CH:22][CH:23]=1>C(Cl)Cl>[Cl:12][C:9]1[CH:10]=[CH:11][C:6]([C:4]2[C:3]3[CH:13]=[CH:14][CH:15]=[CH:16][C:2]=3[NH:1][C:19]3[N:20]=[CH:21][CH:22]=[CH:23][C:18]=3[N:17]=2)=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 761662-Amino-4'-chlorobenzophenoneHCID 805282-Chloro-3-pyridylamine

생성물 1

HCID 1356263936-(4-Chlorophenyl)-11H-pyrido[2,3-b][1,4]benzodiazepine수율 8.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
180 °C

실험 절차

A mixture of 23.2 g (0.10 mole) of 2-amino-4'-chlorobenzophenone and 14.7 g (0.11 mole) of 3-amino-2-chloropyridine (96%) were heated for 1.5 hr at 180° C. under nitrogen atmosphere. The mixture was cooled to room temperature and methylene chloride added. After stirring for 30 min., solids were separated by filtration and triturated in hot 190 proof ethanol. The remaining insoluble material was collected by filtration and recrystallized from benzene-isooctane to give 2.7 g product, m.p. 203°-204.5° C. Drying conditions prior to analyses were: overnight at 97°-98° C./0.1 mm Hg.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. customsolids were separated by filtration
  3. customtriturated in hot 190 proof ethanol
  4. filtrationThe remaining insoluble material was collected by filtration
  5. customrecrystallized from benzene-isooctane

출처 및 근거

ORD 기록
ord-b525a9ed9bd34838b2c385e64d05a04f
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556667

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