Hydrochloric Acid → 1-(2-Chloropyridin-4-yl)piperidin-4-one

HRID 451539ノート

反応式

HRID 451539 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)[CH:5]=[CH:4][N:3]=1.Cl.C(=O)([O-])O.[Na+]>CC(C)=O>[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:17][CH2:16][C:11](=[O:12])[CH2:10][CH2:9]2)[CH:5]=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 866567218-(2-Chloropyridin-4-yl)-1,4-dioxa-8-azaspiro[4.5]decane

生成物 1

HCID 866567191-(2-Chloropyridin-4-yl)piperidin-4-one収率 99%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
50 °C

実験手順

To a solution of 8-(2-chloropyridin-4-yl)-1,4-dioxa-8-azaspiro[4.5]decane (1.26 g, 4.95 mmol) in acetone (11 mL) was added HCl (2 N, 39.6 mL, 79.1 mmol) and the resulting mixture stirred at 50° C. for 2 hours, then cooled to room temperature. The pH was set to ˜8 by adding solid sodium hydrogen carbonate and then extracted with dichloromethane. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated to give the title product (1.03 g, 99%) as a white solid.

後処理

  1. temperaturecooled to room temperature
  2. extractionextracted with dichloromethane
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-f5426199c702457d8b62a4211a4e58cc
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

反応ノート

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