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

HRID 2048122노트

반응식

HRID 2048122 반응식
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]

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-e6f2712cbdc042aa8b87b0407c80cf35
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592629B2

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