Hydrogen chloride-ethyl acetate → 4-chloro-N-[(3R,4R)-3-(3,4-dichlorophenyl)piperidin-4-yl]-N-methylbenzamide Monohydrochloride

HRID 1260944노트

반응식

HRID 1260944 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:10]([CH3:32])[C@@H:11]2[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][C@H:12]2[C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[C:26]([Cl:31])[CH:25]=2)=[O:9])=[CH:4][CH:3]=1.Cl.C(OCC)(=O)C>C(OCC)(=O)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([N:10]([C@@H:11]2[CH2:16][CH2:15][NH:14][CH2:13][C@H:12]2[C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[C:26]([Cl:31])[CH:25]=2)[CH3:32])=[O:9])=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86631351tert-butyl (3R,4R)-4-{[(4-chlorophenyl)carbonyl](methyl)amino}-3-(3,4-dichlorophenyl)piperidine-1-carboxylate

생성물 1

HCID 689287034-chloro-N-[(3R,4R)-3-(3,4-dichlorophenyl)piperidin-4-yl]-N-methylbenzamide Monohydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

To a solution of tert-butyl (3R,4R)-4-{[(4-chlorophenyl)carbonyl](methyl)amino}-3-(3,4-dichlorophenyl)piperidine-1-carboxylate (700 mg) obtained in Example 168 in ethyl acetate (5 mL) was added 4N hydrogen chloride/ethyl acetate solution (5 mL), and the mixture was stirred at 50° C. for 4 hr. The reaction mixture was concentrated under reduced pressure, and the precipitate was collected by filtration to give the title compound.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. filtrationthe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-750d6a6d4a9145bfbe69027bbf0f9325
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08470816B2

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