Potassium Carbonate → HCID 12926609、化合物

HRID 647506ノート

反応式

HRID 647506 の反応式
[C:1]([NH:4][CH:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[Cl:17][C:18]1[CH:23]=[CH:22][CH:21]=[C:20](Cl)[N:19]=1>>[C:1]([NH:4][CH:5]1[CH2:10][CH2:9][N:8]([C:20]2[CH:21]=[CH:22][CH:23]=[C:18]([Cl:17])[N:19]=2)[CH2:7][CH2:6]1)(=[O:3])[CH3:2]

参加物

4

反応物 3

HCID 11430Potassium CarbonateHCID 169892,6-DichloropyridineHCID 14451564-Acetamidopiperidine

生成物 1

HCID 12926609HCID 12926609、化合物収率 78.6%

実験手順

A suspension of 175.5 g of 4-acetamidopiperidine, 269.7 g of potassium carbonate and 182.5 g of 2.6-dichloropyridine in 1600 ml of n.penytylic alcohol is heated at reflux with stirring for 40 hours. The reaction mixture is cooled, the solvent is removed under reduced pressure and the residue is taken up with 100 mlof water. The solid product is extracted with 2000 ml of methylene chloride, the organic phase is washed with water, it is dried over anhydrous sodium sulfate and evaporated to dryness. The residue is taken up with 1200 ml of diisopropylic ether, stirred for 30 minutes, filtered and washed with diisopropylic ether. 246 g of 4-acetamido-1-(6-chloro-2-pyridyl)piperidine are obtained; m.p. 153° to 155° C.

後処理

  1. temperatureis heated
  2. temperatureat reflux
  3. temperatureThe reaction mixture is cooled
  4. customthe solvent is removed under reduced pressure
  5. extractionThe solid product is extracted with 2000 ml of methylene chloride
  6. washthe organic phase is washed with water, it
  7. dry with materialis dried over anhydrous sodium sulfate
  8. customevaporated to dryness
  9. stirringstirred for 30 minutes
  10. filtrationfiltered
  11. washwashed with diisopropylic ether

出典と根拠

ORDレコード
ord-e62a19241dcb486bb33b3f4406268879
出典データセット
uspto-grants-1983_10
特許番号
US04409228

反応ノート

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