Hydrochloric Acid → 4-(Diphenylmethoxy)piperidinium chloride

HRID 465016노트

반응식

HRID 465016 반응식
C(OC([N:6]1[CH2:11][CH2:10][CH:9]([O:12][CH:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:8][CH2:7]1)=O)C.[OH-].[K+].[ClH:28]>C(O)(C)C>[ClH:28].[C:20]1([CH:13]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[O:12][CH:9]2[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]2)[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 10020094Ethyl 4-(diphenylmethoxy)piperidine carboxylate

생성물 1

HCID 441535184-(Diphenylmethoxy)piperidinium chloride수율 71%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A solution of 1-ethoxycarbonyl-4-diphenylmethoxypiperidine (60 g; 0.176 moles) and 85% potassium hydroxide (116 g; 1.76 moles) in isopropanol (600 ml) was boiled under reflux for 6 hours. After cooling, concentrated hydrochloric acid was added until pH=2 and the solvent removed in vacuo. The resulting residue was dissolved in a small quantity of water, washed with diethyl ether and the aqueous solution was made alkaline with aqueous sodium hydroxide solution and extracted with methylene chloride. The organic solution was dried (Na2SO4), the solvent removed in vacuo and the residual oil treated with ethanolic hydrogen chloride solution. 4-Diphenylmethoxy-piperidine hydrochloride (38 g; yield 71%) was obtained.

후처리

  1. temperatureunder reflux for 6 hours
  2. temperatureAfter cooling
  3. customthe solvent removed in vacuo
  4. dissolutionThe resulting residue was dissolved in a small quantity of water
  5. washwashed with diethyl ether
  6. extractionextracted with methylene chloride
  7. dry with materialThe organic solution was dried (Na2SO4)
  8. customthe solvent removed in vacuo
  9. additionthe residual oil treated with ethanolic hydrogen chloride solution

출처 및 근거

ORD 기록
ord-dcb4d11fa0a54c4a8e3b922719fc5c8c
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550116

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