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Sodium Hydroxide → HCID 67312828、化合物

HRID 2190477
ノート
印刷プレビュー

反応式

HRID 2190477 の反応式
[Cl:1][C:2]1[C:10]([C:11]([C:14]#[N:15])([CH3:13])[CH3:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.C(Cl)(=O)C(Cl)=O.[F:22][C:23]1[CH:29]=[CH:28][C:26]([NH2:27])=[CH:25][C:24]=1[O:30][C:31]1[CH:36]=[CH:35][C:34]([N+:37]([O-:39])=[O:38])=[CH:33][CH:32]=1.[OH-].[Na+]>O1CCCC1.C(OCC)(=O)C.O.CN(C)C=O>[Cl:1][C:2]1[C:10]([C:11]([C:14]#[N:15])([CH3:13])[CH3:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([NH:27][C:26]1[CH:28]=[CH:29][C:23]([F:22])=[C:24]([O:30][C:31]2[CH:32]=[CH:33][C:34]([N+:37]([O-:39])=[O:38])=[CH:35][CH:36]=2)[CH:25]=1)=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 14798Sodium HydroxideHCID 65578Oxalyl chlorideHCID 668102752-Chloro-3-(1-cyano-1-methylethyl)benzoic acidHCID 67312965HCID 67312965、化合物

生成物 1

HCID 67312828HCID 67312828、化合物収率 99%

試薬・触媒・溶媒 4

HCID 962Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-chloro-3-(1-cyano-1-methylethyl)benzoic acid (1.98 g, 8.85 mmol) produced in Example A41(ii) in tetrahydrofuran (40 mL) were added oxalyl chloride (1.41 g, 11.1 mmol) and N,N-dimethylformamide (10 μL), and the mixture was stirred for 1 hr. The reaction mixture was concentrated under reduced pressure, and the obtained residue was dissolved in N,N-dimethylacetamide (40 mL). 4-Fluoro-3-(4-nitrophenoxy)aniline (4.69 g, 20.4 mmol) was added, and the mixture was stirred at room temperature for 14 hr. To the reaction mixture were added water (100 ml), 1N aqueous sodium hydroxide solution (50 mL) and ethyl acetate (200 mL). The organic layer was separated, washed with saturated brine (10 mL), and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure to give 2-chloro-3-(1-cyano-1-methylethyl)-N-[4-fluoro-3-(4-nitrophenoxy)phenyl]benzamide (2.01 g, 99%). The obtained compound was used in the next reaction without a further purification.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe obtained residue was dissolved in N,N-dimethylacetamide (40 mL)
  3. stirringthe mixture was stirred at room temperature for 14 hr
  4. customThe organic layer was separated
  5. washwashed with saturated brine (10 mL)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationThe insoluble material was filtered off
  8. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-c0ae00c39a3f442a9859edc602e948f7
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08324395B2

反応ノート

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