Sodium hydride → HCID 59713040、化合物

HRID 2222753ノート

反応式

HRID 2222753 の反応式
[CH3:1][O:2][C:3](=[O:17])[CH:4]([C:6]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[C:8]([F:16])[CH:7]=1)[OH:5].[H-].[Na+].[H][H].F[C:23]1[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:24]=1[C:30]([F:33])([F:32])[F:31]>CN(C)C=O.C(OCC)(=O)C.O>[CH3:1][O:2][C:3](=[O:17])[CH:4]([C:6]1[CH:11]=[C:10]([C:12]([F:14])([F:15])[F:13])[CH:9]=[C:8]([F:16])[CH:7]=1)[O:5][C:25]1[CH:26]=[C:27]([Cl:29])[CH:28]=[CH:23][C:24]=1[C:30]([F:31])([F:32])[F:33]

参加物

8

反応物 4

HCID 24758Sodium hydrideHCID 142277984-Chloro-2-fluoro-1-(trifluoromethyl)benzeneHCID 59713034HCID 59713034、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 59713040HCID 59713040、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

(3-Fluoro-5-trifluoromethyl-phenyl)-hydroxy-acetic acid methyl ester 91 (0.1 mol) was dissolved in dimethylformamide (100 mL) and sodium hydride (0.1 mol) was added. When hydrogen evolution stopped, a solution of 2-fluoro-4-chloro-1-trifluoromethyl-benzene 92 (0.1 mol) in dimethylformamide (25 mL) was added. The progress of the reaction was monitored by TLC. When the reaction was complete, water and ethyl acetate were added. The organic phase was dried and concentrated, and the residue was chromatographed to afford (3-fluoro-5-trifluoromethyl-phenyl)-(5-chloro-2-trifluoromethyl-phenoxy)-acetic acid methyl ester 93. Basic hydrolysis of this compound, as described in Example 1, then afforded the title compound 94.

後処理

  1. customThe organic phase was dried
  2. concentrationconcentrated
  3. customthe residue was chromatographed

出典と根拠

ORDレコード
ord-27a8879c3d184bbf9287c3da7578f548
出典データセット
uspto-grants-2008_05
特許番号
US07371888B2

反応ノート

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