Hydrochloric Acid → Methyl-phenethyl-piperidin-4-YL-amine

HRID 2257134노트

반응식

HRID 2257134 반응식
Cl.[CH3:2][N:3]([CH:12]1[CH2:17][CH2:16][N:15](CC2C=CC=CC=2)[CH2:14][CH2:13]1)[CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[H][H]>C(O)C.O.[C].[Pd]>[CH3:2][N:3]([CH:12]1[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]1)[CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 13784444-[N-methyl-N-(2-phenylethyl)amino]-1-benzylpiperidineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 10856966Methyl-phenethyl-piperidin-4-YL-amine수율 70.1%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

60 ml of concentrated hydrochloric acid and 13.3 g of 10% palladium-carbon were added to a solution of 266 g of 4-[N-methyl-N-(2-phenylethyl)amino]-1-benzylpiperidine in 1 liter of ethanol and 500 ml of water. The mixture was stirred at a hydrogen pressure of 1 atm. at 60° C. for 5 hours. 10% palladium-carbon was removed by filtration and then washed with ethanol. The filtrate and the washings were combined and concentrated under reduced pressure. The residue was added to ice water. The mixture was made alkaline with a 25% aqueous sodium hydroxide solution and then extracted with methylene chloride. The extract was water-washed and then concentrated under reduced pressure. The residue was subjected to vacuum distillation to obtain 131.9 g of 4-[N-methyl-N-(2-phenylethyl)amino]piperidine as a colorless oil.

후처리

  1. custom10% palladium-carbon was removed by filtration
  2. washwashed with ethanol
  3. concentrationconcentrated under reduced pressure
  4. additionThe residue was added to ice water
  5. extractionextracted with methylene chloride
  6. washwashed
  7. concentrationconcentrated under reduced pressure
  8. distillationThe residue was subjected to vacuum distillation

출처 및 근거

ORD 기록
ord-ccaefee9825b4c4a9a5e209782ff7498
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05656642

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