1-Bromo-2-Chloroethane → 1-(2-Chloroethyl)piperidine-4-carbonitrile

HRID 2414123ノート

反応式

HRID 2414123 の反応式
Br[CH2:2][CH2:3][Cl:4].C(=O)([O-])[O-].[K+].[K+].[C:11]([CH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)#[N:12]>C(O)(C)C>[Cl:4][CH2:3][CH2:2][N:16]1[CH2:17][CH2:18][CH:13]([C:11]#[N:12])[CH2:14][CH2:15]1

参加物

5

反応物 3

HCID 78491-Bromo-2-ChloroethaneHCID 11430Potassium CarbonateHCID 1382234-Cyanopiperidine

生成物 1

HCID 110521221-(2-Chloroethyl)piperidine-4-carbonitrile

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

1-Bromo-2-chloroethane (2.6 ml) and potassium carbonate (6.6 g) were added to a solution of 4-cyanopiperidine (2.63 g) in isopropanol (50 ml), followed by refluxing for 10 hours. The reaction mixture was concentrated under reduced pressure. After adding a 50% aqueous solution of potassium carbonate to the residue, the resulting mixture was extracted with diethyl ether. The extract was washed with saturated saline, followed by an addition of anhydrous potassium carbonate to dry the diethyl ether solution. The thus-dried diethyl ether solution was concentrated under reduced pressure. The residue was purified by silica gel chromatography (developer: methanol-chloroform) to obtain 0.31 g of the desired product in an oily form.

後処理

  1. temperatureby refluxing for 10 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionAfter adding a 50% aqueous solution of potassium carbonate to the residue
  4. extractionthe resulting mixture was extracted with diethyl ether
  5. washThe extract was washed with saturated saline
  6. additionfollowed by an addition of anhydrous potassium carbonate
  7. dry with materialto dry the diethyl ether solution
  8. concentrationThe thus-dried diethyl ether solution was concentrated under reduced pressure
  9. customThe residue was purified by silica gel chromatography (developer: methanol-chloroform)

出典と根拠

ORDレコード
ord-01a49f7f7622465398c1f884d08d3fd3
出典データセット
uspto-grants-1988_01
特許番号
US04721788

反応ノート

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