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

HRID 1655017노트

반응식

HRID 1655017 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 186757284-(3,4-Dichlorophenyl)-4-piperidinol수율 90%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e18f70a4f85a4405b8ca44dc72ee84fa
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05410058

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