(3-Methyl-2-nitrophenyl)phenylamine → 3-Methyl-N1-phenylbenzene-1,2-diamine

HRID 242773

反応式

HRID 242773 の反応式
[CH3:1][C:2]1[C:3]([N+:15]([O-])=O)=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:5]=[CH:6][CH:7]=1>CCOC(C)=O.[Pd]>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH:8][C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:3]=1[NH2:15]

参加物

4

反応物 1

HCID 10704534(3-Methyl-2-nitrophenyl)phenylamine

生成物 1

HCID 534243143-Methyl-N1-phenylbenzene-1,2-diamine収率 94.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of (3-methyl-2-nitrophenyl)phenylamine (931 mg, 4.08 mmol) and 10% Pd/C (465 mg) in EtOAc (20 mL) was degassed with a stream of nitrogen and stirred at RT under a hydrogen atmosphere for 4 h. The suspension was then filtered through a PTFE frit and the filtrate was concentrated in vacuo affording 3-Methyl-N1-phenylbenzene-1,2-diamine as an off-white solid (763 mg, 94%). LCMS: RT 3.37 min [M+H]+ 199.0.

後処理

  1. customwas degassed with a stream of nitrogen
  2. filtrationThe suspension was then filtered through a PTFE frit
  3. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-408d99b9bd6c4aecafa90e89800a1cce
出典データセット
uspto-grants-2014_02
特許番号
US08653089B2

関連ノート

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