Potassium Hydroxide → 5-(2-Fluorophenoxy)-2-pyrazinecarboxylic acid

HRID 340092ノート

反応式

HRID 340092 の反応式
C[O:2][C:3]([C:5]1[CH:10]=[N:9][C:8]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[F:18])=[CH:7][N:6]=1)=[O:4].[OH-].[K+]>C(O)C>[F:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[O:11][C:8]1[N:9]=[CH:10][C:5]([C:3]([OH:4])=[O:2])=[N:6][CH:7]=1

参加物

4

実験手順

5-(2-Fluoro-phenoxy)-pyrazine-2-carboxylic acid methyl ester (Preparation 44, 57.9 g, 233 mmol) was added to a solution of KOH (15 g, 267 mmol) in 78% ethanol (330 mL). The solution was stirred at room temperature for 18 hours, and the formed precipitate was collected by filtration. The resulting solid was dissolved in water (200 mL), and the solution was acidified with aqueous hydrochloric acid. The formed precipitate was collected by filtration, dried and recrystallised from 41% ethanol (265 mL) to give the title compound (28.3 g, 120.8 mmol) in 51.8% yield.

後処理

  1. filtrationthe formed precipitate was collected by filtration
  2. dissolutionThe resulting solid was dissolved in water (200 mL)
  3. filtrationThe formed precipitate was collected by filtration
  4. customdried
  5. customrecrystallised from 41% ethanol (265 mL)

出典と根拠

ORDレコード
ord-318af253e5ac47f987cfe7f46a9f65f9
出典データセット
uspto-grants-2014_11
特許番号
US08895544B2

反応ノート

読み込み中…