4-(Methylamino)benzoic acid → Cis-4-(methylamino)cyclohexanecarboxylic acid

HRID 2295293

反応式

HRID 2295293 の反応式
[CH3:1][NH:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=1.[H][H]>[Rh].O>[CH3:1][NH:2][CH:3]1[CH2:11][CH2:10][CH:6]([C:7]([OH:9])=[O:8])[CH2:5][CH2:4]1

参加物

5

反応物 2

HCID 663454-(Methylamino)benzoic acidHCID 178418361HCID 178418361、化合物

生成物 1

HCID 429561Cis-4-(methylamino)cyclohexanecarboxylic acid収率 75%

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒HCID 962Water溶媒

実験手順

A slurry of 33.0 g (0.218 m) of 4-(methylamino)benzoic acid and 4.0 g of 5% rhodium on alumina catalyst in 350 ml of water was shaken under 1500 psig of hydrogen for 24 hours. The insolubles were removed by filtration. The slurry from partial removal of water under reduced pressure was diluted with 300 ml of N,N-dimethylformamide and chilled. The precipitated solid was filtered, washed with several portions of cold acetone, and dried to yield 23 g (75%) of 4-(methylamino)cyclohexanecarboxylic acid.

後処理

  1. customThe insolubles were removed by filtration
  2. customThe slurry from partial removal of water under reduced pressure
  3. additionwas diluted with 300 ml of N,N-dimethylformamide
  4. temperaturechilled
  5. filtrationThe precipitated solid was filtered
  6. washwashed with several portions of cold acetone
  7. customdried

出典と根拠

ORDレコード
ord-58d2685837484985a77bef64d1f51f42
出典データセット
uspto-grants-1984_01
特許番号
US04424213

関連ノート

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