Potassium Carbonate → (S)-tert-Butyl 5-chloro-4-((5-chloro-6-((1,1,1-trifluoropropan-2-yl)oxy)pyridin-3-yl)oxy)-2-fluorobenzoate

HRID 2048121ノート

反応式

HRID 2048121 の反応式
[Cl:1][C:2]1[C:3](F)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8].[Cl:17][C:18]1[CH:19]=[C:20]([OH:31])[CH:21]=[N:22][C:23]=1[O:24][C@@H:25]([CH3:30])[C:26]([F:29])([F:28])[F:27].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[Cl:1][C:2]1[C:3]([O:31][C:20]2[CH:21]=[N:22][C:23]([O:24][C@@H:25]([CH3:30])[C:26]([F:29])([F:28])[F:27])=[C:18]([Cl:17])[CH:19]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 580424575-chloro-6-[(1S)-2,2,2-trifluoro-1-methylethoxy]pyridin-3-olHCID 58042499Tert-butyl 5-chloro-2,4-difluorobenzoate

生成物 1

HCID 58042393(S)-tert-Butyl 5-chloro-4-((5-chloro-6-((1,1,1-trifluoropropan-2-yl)oxy)pyridin-3-yl)oxy)-2-fluorobenzoate収率 58.6%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

tert-Butyl 5-chloro-2,4-difluorobenzoate (Preparation 59, 8.3 g, 33.4 mmol) was added to a solution of 5-chloro-6-[(1S)-2,2,2-trifluoro-1-methylethoxy]pyridin-3-ol (Preparation 231, 16.2 g, 66.8 mmol) and potassium carbonate (27.8 g, 200 mmol) in dimethyl sulfoxide (100 mL). The reaction mixture was stirred at room temperature for 18 hours then quenched with an aqueous solution of sodium hydroxide (1 M, 100 mL). A white precipitate formed and was collected by filtration to give the title compound as a white solid (9.2 g).

後処理

  1. customthen quenched with an aqueous solution of sodium hydroxide (1 M, 100 mL)
  2. customA white precipitate formed
  3. filtrationwas collected by filtration

出典と根拠

ORDレコード
ord-d068bf8968dc4366997578e0602ec724
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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