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Ammonium Chloride → 5-chloro-2-(3,4,5-trifluorophenyl)pentanoic acid N'-{(E)-3-[2-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acryloyl}hydrazide

HRID 546676
ノート
印刷プレビュー

反応式

HRID 546676 の反応式
C(N(C(C)C)CC)(C)C.C1N(P(Cl)(N2C(=O)OCC2)=O)C(=O)OC1.Cl.[Cl:26][CH2:27][CH2:28][CH2:29][CH:30]([C:35]1[CH:40]=[C:39]([F:41])[C:38]([F:42])=[C:37]([F:43])[CH:36]=1)[C:31]([NH:33][NH2:34])=[O:32].[F:44][C:45]1[CH:50]=[C:49]([N:51]2[CH:55]=[C:54]([CH3:56])[N:53]=[CH:52]2)[C:48]([O:57][CH3:58])=[CH:47][C:46]=1/[CH:59]=[CH:60]/[C:61](O)=[O:62].[Cl-].[NH4+]>C(Cl)Cl.C(OCC)(=O)C>[F:44][C:45]1[CH:50]=[C:49]([N:51]2[CH:55]=[C:54]([CH3:56])[N:53]=[CH:52]2)[C:48]([O:57][CH3:58])=[CH:47][C:46]=1/[CH:59]=[CH:60]/[C:61]([NH:34][NH:33][C:31](=[O:32])[CH:30]([C:35]1[CH:36]=[C:37]([F:43])[C:38]([F:42])=[C:39]([F:41])[CH:40]=1)[CH2:29][CH2:28][CH2:27][Cl:26])=[O:62]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 152842Bis(2-oxo-3-oxazolidinyl)phosphinic chlorideHCID 66839107HCID 66839107、化合物HCID 668392315-Chloro-2-(3,4,5-trifluorophenyl)pentanoic acid hydrazide hydrochloride

生成物 1

HCID 66839536
5-chloro-2-(3,4,5-trifluorophenyl)pentanoic acid N'-{(E)-3-[2-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acryloyl}hydrazide
収率 103.6%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

IPEA (0.31 mL) and BOPCl (119 mg) were added to a solution of 5-chloro-2-(3,4,5-trifluorophenyl)pentanoic acid hydrazide hydrochloride (114 mg) and (E)-3-[2-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acrylic acid (99 mg) in methylene chloride (5 mL), and the reaction solution was stirred at room temperature for one hour. Ethyl acetate and a saturated ammonium chloride solution were added to the reaction solution, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 200 mg of the title compound. The property value of the compound is as follows.

後処理

  1. customthe organic layer was separated
  2. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-20531ba26a4b4890ad9c61aa4b5b3a19
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07935815B2

反応ノート

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