Hydrochloric Acid → 4-(Diphenylmethoxy)piperidinium chloride

HRID 465016ノート

反応式

HRID 465016 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 441535184-(Diphenylmethoxy)piperidinium chloride収率 71%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dcb4d11fa0a54c4a8e3b922719fc5c8c
出典データセット
uspto-grants-1985_10
特許番号
US04550116

反応ノート

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