Ammonia → 1-(Cyclohexylmethyl)piperidin-4-amine

HRID 261049노트

반응식

HRID 261049 반응식
[CH:1]1([CH2:7][N:8]2[CH2:13][CH2:12][C:11](=O)[CH2:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[NH3:15]>[Ni]>[CH:1]1([CH2:7][N:8]2[CH2:13][CH2:12][CH:11]([NH2:15])[CH2:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 119596651-(Cyclohexylmethyl)piperidin-4-one

생성물 1

HCID 64969411-(Cyclohexylmethyl)piperidin-4-amine

시약·촉매·용매 1

HCID 935Nickel촉매

실험 절차

A solution of 1-cyclohexylmethylpiperid-4-one (65 g; 0.33 moles in a saturated ethanolic solution of ammonia (350 ml) was hydrogenated in the presence of Raney nickel catalyst (6.5 g) at 75° C. and 13 atmospheres for 3.5 hours. The mixture was cooled, the catalyst filtered off and the solvent removed by distillation in vacuo. The residue was treated with a saturated ethanolic solution of hydrogen chloride, and the insoluble dihydrochloride was filtered off, treated with an aqueous solution of sodium hydroxide and extracted with chloroform. The organic layer was dried (Na2SO4) and the solvent removed in vacuo giving 1-cyclohexylmethyl-4-aminopiperidine (45.5 g) as a viscous liquid, b.p. 105°-110° C./0.3 mm Hg.

후처리

  1. temperatureThe mixture was cooled
  2. filtrationthe catalyst filtered off
  3. customthe solvent removed by distillation in vacuo
  4. additionThe residue was treated with a saturated ethanolic solution of hydrogen chloride
  5. filtrationthe insoluble dihydrochloride was filtered off
  6. additiontreated with an aqueous solution of sodium hydroxide
  7. extractionextracted with chloroform
  8. dry with materialThe organic layer was dried (Na2SO4)
  9. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-5ead671b13004a0ba7607c817d8df21a
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04163789

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