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

HRID 261049ノート

反応式

HRID 261049 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 64969411-(Cyclohexylmethyl)piperidin-4-amine

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5ead671b13004a0ba7607c817d8df21a
出典データセット
uspto-grants-1979_08
特許番号
US04163789

反応ノート

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