Hydrochloric Acid → 4-Piperidinamine, 1-(1-phenylcyclohexyl)-

HRID 1654445ノート

反応式

HRID 1654445 の反応式
[C:1]1([C:7]2([N:13]3[CH2:18][CH2:17][C:16](=O)[CH2:15][CH2:14]3)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])(=O)C.[NH4+].C([BH3-])#[N:26].[Na+].Cl.C(=O)([O-])[O-].[K+].[K+]>CO.O>[NH2:26][CH:16]1[CH2:17][CH2:18][N:13]([C:7]2([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[CH2:14][CH2:15]1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 4250911-(1-Phenylcyclohexyl)piperidin-4-oneHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydride

生成物 1

HCID 110543604-Piperidinamine, 1-(1-phenylcyclohexyl)-

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

1-(1-phenylcyclohexyl)-4-piperidone (0.245 g) and ammonium acetate (1 g) were dissolved in 3.5 mL dry methanol. After stirring at room temperature for 10 minutes, sodium cyanoborohydride (0.1 g) was added and the reaction was stoppered. After 20 hours, 0.1 mL of concentrated hydrochloric acid was added followed by 10 mL water and the mixture was stirred for 1.5 hours. The solution was basified with potassium carbonate to pH 9 and extracted with methylene chloride. The methylene chloride was dried over Na2SO4 and removed in vacuo. The product distilled as a colorless, clear oil at 90-130° C. in vacuo (about 5 mmHg).

後処理

  1. waitAfter 20 hours
  2. stirringthe mixture was stirred for 1.5 hours
  3. extractionextracted with methylene chloride
  4. dry with materialThe methylene chloride was dried over Na2SO4
  5. customremoved in vacuo
  6. distillationThe product distilled as a colorless, clear oil at 90-130° C. in vacuo (about 5 mmHg)

出典と根拠

ORDレコード
ord-4df8efb526da402ba229fa2e06c19e4e
出典データセット
uspto-grants-1995_04
特許番号
US05407834

反応ノート

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