Trifluoroacetic acid → 5-Chloro-4-(((5-chloro-6-cyclopropylpyridin-3-yl)oxy)methyl)-2-fluorobenzoic acid

HRID 1525676ノート

反応式

HRID 1525676 の反応式
[Cl:1][C:2]1[C:3]([CH2:16][O:17][C:18]2[CH:19]=[N:20][C:21]([CH:25]3[CH2:27][CH2:26]3)=[C:22]([Cl:24])[CH:23]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([O:9]C(C)(C)C)=[O:8].C(O)(C(F)(F)F)=O>ClCCl>[Cl:1][C:2]1[C:3]([CH2:16][O:17][C:18]2[CH:19]=[N:20][C:21]([CH:25]3[CH2:27][CH2:26]3)=[C:22]([Cl:24])[CH:23]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([OH:9])=[O:8]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 89633279HCID 89633279、化合物

生成物 1

HCID 896191735-Chloro-4-(((5-chloro-6-cyclopropylpyridin-3-yl)oxy)methyl)-2-fluorobenzoic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of tert-butyl 5-chloro-4-(((5-chloro-6-cyclopropylpyridin-3-yl)oxy)methyl)-2-fluorobenzoate (Preparation 26, 1.24 g, 3.01 mmol) in dichloromethane (22 mL) was added TFA (10.0 mL, 0.02 mol). The mixture was stirred under nitrogen at room temperature for 18 hours. Additional TFA (2.50 mL, 32.0 mmol) was added and stirring continued for 3 hours. The reaction mixture was evaporated under reduced pressure and the resulting residue dissolved in EtOAc (25 mL) and washed with 2M aqueous solution of HCl (25 mL). The resulting solid was filtered to afford the title compound (1.4 g, crude quant.) which was used with no further purification.

後処理

  1. stirringstirring
  2. waitcontinued for 3 hours
  3. customThe reaction mixture was evaporated under reduced pressure
  4. dissolutionthe resulting residue dissolved in EtOAc (25 mL)
  5. washwashed with 2M aqueous solution of HCl (25 mL)
  6. filtrationThe resulting solid was filtered

出典と根拠

ORDレコード
ord-e73b0d51730a4acc91d74722f1d80874
出典データセット
uspto-grants-2015_07
特許番号
US09085517B2

反応ノート

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