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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
ノート
印刷プレビュー

反応式

HRID 1260932 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetate2 回HCID 86631298HCID 86631298、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c6b0e2f86ba040f3a81ab71411cca828
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08470816B2

反応ノート

読み込み中…

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