O-Xylene → 2-Amino-4'-chlorobiphenyl

HRID 534710ノート

反応式

HRID 534710 の反応式
C1(C)C(C)=CC=CC=1.[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[N+:22]([O-])=O)=[CH:12][CH:11]=1>[Pt].CC(C)=O>[Cl:9][C:10]1[CH:11]=[CH:12][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[NH2:22])=[CH:14][CH:15]=1

参加物

5

反応物 2

HCID 7237O-XyleneHCID 2355494'-Chloro-2-nitro-1,1'-biphenyl

生成物 1

HCID 2622612-Amino-4'-chlorobiphenyl

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 180Acetone溶媒

反応条件

温度
100 °C

実験手順

In a 20 ml autoclave were placed 1 g of xylene, 6 mg of a Pt/C catalyst (containing 1% by weight of Pt with respect to the weight of carbon) and 0.25 g (1 mmol) of 4′-chloro-2-nitrobiphenyl obtained in example 1.4. The mixture was stirred under hydrogen pressure (7-8 bar) at 100° C. until the starting material had disappeared (monitoring via HPLC). After completion of the reaction the mixture was cooled to ambient temperature and diluted with 15 ml of acetone. The catalyst was filtered off and the filtrate was evaporated in vacuo yielding 0.2 g (91% of theory) of the title compound in a purity of 93% (HPLC % by weight).

後処理

  1. customAfter completion of the reaction the mixture
  2. temperaturewas cooled to ambient temperature
  3. filtrationThe catalyst was filtered off
  4. customthe filtrate was evaporated in vacuo

出典と根拠

ORDレコード
ord-7edf882425b346a5b8725fcdced879a2
出典データセット
uspto-grants-2014_10
特許番号
US08853455B2

反応ノート

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