Potassium Hydroxide → 4-(3,4-Dichlorophenyl)-4-piperidinol

HRID 5155ノート

反応式

HRID 5155 の反応式
C(OC([N:6]1[CH2:11][CH2:10][C:9]([OH:20])([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[CH2:8][CH2:7]1)=O)C.[OH-].[K+]>C(O)CCC>[OH:20][C:9]1([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 20077503Ethyl 4-(3,4-dichlorophenyl)-4-hydroxypiperidine-1-carboxylate

生成物 1

HCID 186757284-(3,4-Dichlorophenyl)-4-piperidinol収率 90%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of 64.2 g of 1-ethoxycarbonyl-4-hydroxy-4-(3,4-dichlorophenyl)piperidine (X-1) and a solution of 72.4 g of KOH in 700 ml of nBuOH is refluxed for 2 hours and evaporated. The reaction mixture is concentrated under reduced pressure and extracted with ethyl acetate. The organic layer is washed with water, dried and evaporated. The resulting crystalline residue is recrystallized from ethyl acetate to prepare 44.7 g (Yield: 90.0%) of the compound (II-1). mp. 144.5°-146.0° C.

後処理

  1. customevaporated
  2. concentrationThe reaction mixture is concentrated under reduced pressure
  3. extractionextracted with ethyl acetate
  4. washThe organic layer is washed with water
  5. customdried
  6. customevaporated
  7. customThe resulting crystalline residue is recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-0d60770bcb50476997f7e87cec0a58de
出典データセット
uspto-grants-1993_09
特許番号
US05243051

反応ノート

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