4-Hydroxypiperidine-1-carbonitrile → 1-(3-Isopropyl-1,2,4-oxadiazol-5-YL)piperidin-4-OL

HRID 68788

反応式

HRID 68788 の反応式
[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]#[N:9])[CH2:4][CH2:3]1.[OH:10][NH:11][C:12](=N)[CH:13]([CH3:15])[CH3:14]>C(OCC)(=O)C.CCOCC.[Cl-].[Cl-].[Zn+2]>[CH3:14][CH:13]([C:12]1[N:9]=[C:8]([N:5]2[CH2:6][CH2:7][CH:2]([OH:1])[CH2:3][CH2:4]2)[O:10][N:11]=1)[CH3:15]

参加物

6

反応物 2

HCID 218978254-Hydroxypiperidine-1-carbonitrileHCID 178449908HCID 178449908、化合物

生成物 1

HCID 218977441-(3-Isopropyl-1,2,4-oxadiazol-5-YL)piperidin-4-OL

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒HCID 3283Diethyl Ether溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

4-Hydroxypiperidine-1-carbonitrile (3.0 g) and N-hydroxy-2-methylpropanimidamide (2.9 g) are dissolved in ethyl acetate (20 ml) and 1 M ZnCl2 in Et2O (29 ml) is added. A precipitate forms and the solvent is decanted off. Additional Et2O (20 ml) is added to wash the precipitate and again is decanted off. Ethanol (20 ml) is added followed by concentrated aqueous HCl (7.5 ml) and the mixture is heated to 100° C. for 3.5 h.

後処理

  1. customA precipitate forms and the solvent is decanted off
  2. additionAdditional Et2O (20 ml) is added
  3. washto wash the precipitate
  4. customagain is decanted off
  5. additionEthanol (20 ml) is added

出典と根拠

ORDレコード
ord-7965278f0abf44a5b7fbd8f75fc4af5e
出典データセット
uspto-grants-2014_09
特許番号
US08822471B2

関連ノート

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