Trifluoroacetic acid → HCID 58042402、化合物

HRID 2048116ノート

反応式

HRID 2048116 の反応式
[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:18]=[N:19][C:20]([CH:24]3[CH2:26][CH2:25]3)=[C:21]([Cl:23])[CH:22]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([O:9]C(C)(C)C)=[O:8].FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:18]=[N:19][C:20]([CH:24]3[CH2:25][CH2:26]3)=[C:21]([Cl:23])[CH:22]=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 acidHCID 58042480HCID 58042480、化合物

生成物 1

HCID 58042402HCID 58042402、化合物収率 97%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
45 °C

実験手順

To a solution of tert-butyl 5-chloro-4-[(5-chloro-6-cyclopropylpyridin-3-yl)oxy]-2-fluorobenzoate (Preparation 264, 54.0 g, 135.59 mmol) in dichloromethane (270 mL) was added trifluoroacetic acid (30.76 mL, 406.77 mmol). The resulting solution was heated at 45° C. for 24 hours and concentrated under reduced pressure at 45° C. tert Butyl methyl ether (100 mL) was added to the residue and the resulting slurry stirred at room temperature for 2.5 hours, filtered, washed with tert butyl methyl ether (20 mL) and dried to give the title compound as an off-white solid (45.0 g, 97%).

後処理

  1. concentrationconcentrated under reduced pressure at 45° C. tert Butyl methyl ether (100 mL)
  2. additionwas added to the residue
  3. filtrationfiltered
  4. washwashed with tert butyl methyl ether (20 mL)
  5. customdried

出典と根拠

ORDレコード
ord-6aa7c4dcabb942ceb29551a63a210785
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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