N-Methyl-3-nitroaniline → N1-Methylbenzene-1,3-diamine

HRID 2254014ノート

反応式

HRID 2254014 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-])=O)[CH:4]=1>C(O)C.[Pd]>[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([NH2:9])[CH:4]=1

参加物

4

反応物 1

HCID 219622N-Methyl-3-nitroaniline

生成物 1

HCID 5151957N1-Methylbenzene-1,3-diamine収率 96%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

8 g of the precipitate was dissolved in 20 mL of 95% ethanol, 1 g of a catalyst having 5 wt. % Pd on a carbon support was added and hydrogenation of the N-methyl-3-nitroaniline was carried out at 50 psig (337 kPa gage) for about 10 minutes, during which time the temperature increased to about 70° C. The hydrogenated mixture was cooled to room temperature, filtered to recover the solids, which were then washed with methanol and the liquid filtrates combined. Finally, the liquids were concentrated under vacuum and distilled through a short path Kugelrohr oven at about 140° C. and 3 torr to produce a 96% yield of N-methyl m-phenylenediamine.

後処理

  1. additionwas added
  2. temperatureThe hydrogenated mixture was cooled to room temperature
  3. filtrationfiltered
  4. customto recover the solids, which
  5. washwere then washed with methanol
  6. concentrationFinally, the liquids were concentrated under vacuum
  7. distillationdistilled through a short path Kugelrohr oven at about 140° C.

出典と根拠

ORDレコード
ord-c1390334349e4e319cc0af1081c1e4f5
出典データセット
uspto-grants-1993_08
特許番号
US05234598

反応ノート

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