Hydrochloric Acid → 1-Benzoylpiperidine-4-carboxylic acid

HRID 617192

반응식

HRID 617192 반응식
[NH:1]1[CH2:9][CH2:8][CH:4]([C:5]([OH:7])=[O:6])[CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[C:16](Cl)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.Cl>O>[C:16]([N:1]1[CH2:9][CH2:8][CH:4]([C:5]([OH:7])=[O:6])[CH2:3][CH2:2]1)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 37734-Piperidinecarboxylic acidHCID 7412Benzoyl chlorideHCID 11430Potassium Carbonate

생성물 1

HCID 789351-Benzoylpiperidine-4-carboxylic acid수율 95%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To an ice cold solution of isonipecotic acid (90 g, 0.697 mol) and potassium carbonate (81 g, 1.31 mol) in water (1.3 liter) was added dropwise benzoyl chloride (81 ml, 0.697 mol) over a period of about an hour at about 5° C. The mixture was stirred at room temperature overnight. The reaction mixture was acidified with 6N hydrochloric acid and extracted with dichloromethane. The organic layer was washed with water and then dried over magnesium sulfate and the solvent was evaporated in vacuo. Crystallization from isopropyl alcohol-diethyl ether to give the titled compound (154.4 g).

후처리

  1. extractionextracted with dichloromethane
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was evaporated in vacuo
  5. customCrystallization from isopropyl alcohol-diethyl ether

출처 및 근거

ORD 기록
ord-090031d131f24188b7adc55f41b6ba9b
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05948786

연결된 노트

불러오는 중…