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

HRID 451539노트

반응식

HRID 451539 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f5426199c702457d8b62a4211a4e58cc
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

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