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

HRID 1602881ノート

反応式

HRID 1602881 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-11bcf332410b4858aeea2cfc2f63767d
出典データセット
uspto-grants-1999_11
特許番号
US05985875

反応ノート

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