Ammonia → 4-[4-(4-Chlorobenzoyl)benzyl]-3,5-dichloroaniline

HRID 1602881노트

반응식

HRID 1602881 반응식
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([C:6]([C:8]2[CH:25]=[CH:24][C:11]([CH2:12][C:13]3[C:18]([Cl:19])=[CH:17][C:16]([N+:20]([O-])=O)=[CH:15][C:14]=3[Cl:23])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.N>C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([C:8]2[CH:25]=[CH:24][C:11]([CH2:12][C:13]3[C:18]([Cl:19])=[CH:17][C:16]([NH2:20])=[CH:15][C:14]=3[Cl:23])=[CH:10][CH:9]=2)=[O:7])=[CH:26][CH:27]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 196083034-[4-(4-Chlorobenzoyl)benzyl]-3,5-dichloronitrobenzene

생성물 1

HCID 196083004-[4-(4-Chlorobenzoyl)benzyl]-3,5-dichloroaniline수율 70%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

In 50 ml of ethyl acetate was dissolved 3.25 g of 4-[4-(4-chlorobenzoyl)benzyl]-3,5-dichloronitrobenzene, and 8.00 g of SnCl3.2H2O was added. The reaction mixture was refluxed for 1 hour, and then poured into ice-water. The mixture was alkalified with conc. ammonia solution, and the organic layer was collected by decantation. The aqueous layer was extracted twice with 50 ml of ethyl acetate, and the organic layers were combined, washed with water, dried and concentrated. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/2) to give the above-identified compound as pale brown amorphous powder (yield: 70%).

후처리

  1. additionwas added
  2. temperatureThe reaction mixture was refluxed for 1 hour
  3. customthe organic layer was collected by decantation
  4. extractionThe aqueous layer was extracted twice with 50 ml of ethyl acetate
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/2)

출처 및 근거

ORD 기록
ord-11bcf332410b4858aeea2cfc2f63767d
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05985875

반응 노트

불러오는 중…