Hydrochloric Acid → 1-(4-Hydroxypiperidin-1-yl)cyclohexane-1-carbonitrile

HRID 466260

反応式

HRID 466260 の反応式
O[N:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.Cl.[C:9]1(=O)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.[C-:16]#[N:17].[K+].[OH2:19]>>[C:16]([C:9]1([N:2]2[CH2:7][CH2:6][CH:5]([OH:19])[CH2:4][CH2:3]2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)#[N:17]

参加物

6

反応条件

温度
0 °C

実験手順

4 hydroxypiperidine (Aldrich Chemical Co., Inc., supra) (5q) was dissolved in distilled water (14 mL), cooled to 0° C. and the pH was adjusted to between 4 and 5 by addition of concentrated hydrochloric acid and 4 hydroxypiperidine. After warming to room temperature, 5.2 mL cyclohexanone and 3.3 g potassium cyanide in water (9 mL) were added sequentially. After 18 hours of stirring at room temperature, the solid was filtered. The solid was dissolved in 100 mL methylene chloride, dried over Na2SO4, filtered and the solvent was removed in vacuo to yield pure 1 (1 cyanocyclohexyl) 4 hydroxypiperidine.

後処理

  1. temperatureAfter warming to room temperature
  2. filtrationthe solid was filtered
  3. dissolutionThe solid was dissolved in 100 mL methylene chloride
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-a4eb416b22e64863aba5506a62cab93e
出典データセット
uspto-grants-1992_10
特許番号
US05155212

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