盐酸 → 4-Piperidinamine, 1-(1-phenylcyclohexyl)-

HRID 893403笔记

反应方程式

HRID 893403 反应方程式
[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

参与物

8

反应物 5

HCID 313盐酸HCID 11430碳酸钾HCID 4250911-(1-Phenylcyclohexyl)piperidin-4-oneHCID 517165乙酸铵HCID 5003444氰基硼氢化钠

产物 1

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

试剂、催化剂与溶剂 2

HCID 887Methanol溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

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).

后处理

  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)

来源与证据

ORD记录
ord-10e995c635c64877949570e7d4c5a91e
来源数据集
uspto-grants-1992_06
专利号
US05124457

反应笔记

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