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

HRID 1588223노트

반응식

HRID 1588223 반응식
[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

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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 stoppered. After 20 hours, 0.1 ml 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).

후처리

  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)

출처 및 근거

ORD 기록
ord-41e8c88c76dc42d184ec29f53c2ce388
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05221629

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