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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrogen chloride-ethyl acetate → N-[(3R,4R)-3-(3,4-dichlorophenyl)-1-(piperidin-4-ylcarbonyl)piperidin-4-yl]-N-methyl-3,5-bis(trifluoromethyl)benzamide Monohydrochloride

HRID 1260932
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HRID 1260932 반응식
[F:1][C:2]([F:47])([F:46])[C:3]1[CH:4]=[C:5]([C:13]([N:15]([CH3:45])[C@@H:16]2[CH2:21][CH2:20][N:19]([C:22]([CH:24]3[CH2:29][CH2:28][N:27](C(OC(C)(C)C)=O)[CH2:26][CH2:25]3)=[O:23])[CH2:18][C@H:17]2[C:37]2[CH:42]=[CH:41][C:40]([Cl:43])=[C:39]([Cl:44])[CH:38]=2)=[O:14])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.Cl.C(OCC)(=O)C>C(OCC)(=O)C>[ClH:43].[Cl:44][C:39]1[CH:38]=[C:37]([C@H:17]2[C@H:16]([N:15]([CH3:45])[C:13](=[O:14])[C:5]3[CH:6]=[C:7]([C:9]([F:11])([F:10])[F:12])[CH:8]=[C:3]([C:2]([F:46])([F:1])[F:47])[CH:4]=3)[CH2:21][CH2:20][N:19]([C:22]([CH:24]3[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]3)=[O:23])[CH2:18]2)[CH:42]=[CH:41][C:40]=1[Cl:43]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetate2회HCID 86631298HCID 86631298, 화합물

생성물 1

HCID 86631339N-[(3R,4R)-3-(3,4-dichlorophenyl)-1-(piperidin-4-ylcarbonyl)piperidin-4-yl]-N-methyl-3,5-bis(trifluoromethyl)benzamide Monohydrochloride수율 177.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
50 °C

실험 절차

To a solution of tert-butyl 4-{[(3R,4R)-4-[{[3,5-bis(trifluoromethyl)phenyl]carbonyl}(methyl)amino]-3-(3,4-dichlorophenyl)piperidin-1-yl]carbonyl}piperidine-1-carboxylate (0.502 g) obtained in Example 87 in ethyl acetate (5 mL) was added 4N hydrogen chloride/ethyl acetate (4 mL), and the mixture was stirred at 50° C. for 2 hr. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in ethyl acetate. This was washed with 1N aqueous sodium hydroxide solution and dried, and the solvent was evaporated under reduced pressure. The obtained residue was treated with 1 equivalent of 4N hydrogen chloride/ethyl acetate to give the title compound (0.405 g, 89%) as a white powder.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThis was washed with 1N aqueous sodium hydroxide solution
  4. customdried
  5. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-c6b0e2f86ba040f3a81ab71411cca828
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08470816B2

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