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

HRID 464647

반응식

HRID 464647 반응식
[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

참가 물질

5

반응물 2

HCID 663454-(Methylamino)benzoic acidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 429561Cis-4-(methylamino)cyclohexanecarboxylic acid수율 75%

시약·촉매·용매 2

HCID 23948Rhodium촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1abd61c4c37a44ee91023e6cb152d183
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04548929

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