Trifluoroacetic acid → (S)-5-chloro-4-((5-chloro-6-((1,1,1-trifluoropropan-2-yl)oxy)pyridin-3-yl)oxy)-2-fluorobenzoic acid

HRID 2048122ノート

反応式

HRID 2048122 の反応式
FC(F)(F)C(O)=O.[Cl:8][C:9]1[C:10]([O:23][C:24]2[CH:25]=[N:26][C:27]([O:31][C@@H:32]([CH3:37])[C:33]([F:36])([F:35])[F:34])=[C:28]([Cl:30])[CH:29]=2)=[CH:11][C:12]([F:22])=[C:13]([CH:21]=1)[C:14]([O:16]C(C)(C)C)=[O:15]>ClCCl>[Cl:8][C:9]1[C:10]([O:23][C:24]2[CH:25]=[N:26][C:27]([O:31][C@@H:32]([CH3:37])[C:33]([F:35])([F:36])[F:34])=[C:28]([Cl:30])[CH:29]=2)=[CH:11][C:12]([F:22])=[C:13]([CH:21]=1)[C:14]([OH:16])=[O:15]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 58042393(S)-tert-Butyl 5-chloro-4-((5-chloro-6-((1,1,1-trifluoropropan-2-yl)oxy)pyridin-3-yl)oxy)-2-fluorobenzoate

生成物 1

HCID 58042412(S)-5-chloro-4-((5-chloro-6-((1,1,1-trifluoropropan-2-yl)oxy)pyridin-3-yl)oxy)-2-fluorobenzoic acid収率 85%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (4.4 mL, 58.7 mmol) was added to a solution of (S)-tert-butyl 5-chloro-4-((5-chloro-6-((1,1,1-trifluoropropan-2-yl)oxy)pyridin-3-yl)oxy)-2-fluorobenzoate (Preparation 298, 9.2 g, 19.6 mmol) in dichloromethane (50 mL). The reaction mixture was stirred at room temperature for 20 hours then concentrated in vacuo. The crude was purified by silica gel chromatography, eluting with heptane:ethyl acetate (from 95:5 to 40:60), to provide the title compound as a white solid (6.9 g, 85%).

後処理

  1. concentrationthen concentrated in vacuo
  2. customThe crude was purified by silica gel chromatography
  3. washeluting with heptane

出典と根拠

ORDレコード
ord-e6f2712cbdc042aa8b87b0407c80cf35
出典データセット
uspto-grants-2013_11
特許番号
US08592629B2

反応ノート

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