Methanol → 4-Chloro-2-cyclopropylamino-5-fluoro-benzoic acid
反応式
C([O:3][C:4](=[O:17])[C:5]1[CH:10]=[C:9]([F:11])[C:8]([Cl:12])=[CH:7][C:6]=1[NH:13][CH:14]1[CH2:16][CH2:15]1)C.[Li+].[OH-].CO>C1COCC1>[Cl:12][C:8]1[C:9]([F:11])=[CH:10][C:5]([C:4]([OH:17])=[O:3])=[C:6]([NH:13][CH:14]2[CH2:15][CH2:16]2)[CH:7]=1参加物
5
実験手順
A solution of 4-chloro-2-cyclopropylamino-5-fluoro-benzoic acid ethyl ester (Example B-3, 4.10 g, 15.9 mmol) in THF (100 mL) was reacted with an aqueous solution of 1.0 N LiOH (45 mL, 45 mmol) and methanol (40 mL) and allowed to stir overnight. The mixture was then concentrated to one-third volume and acidified with 1.0 N HCl. The mixture was extracted with ethyl acetate. the organic layers combined, dried with sodium sulfate, and concentrated to provide 3.0 g of the title compound as an oil.
後処理
- concentrationThe mixture was then concentrated to one-third volume
- extractionThe mixture was extracted with ethyl acetate
- dry with materialdried with sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-d9d12f465747472eaa14154960d0876d
- 出典データセット
- uspto-grants-2001_12
- 特許番号
- US06331538B1
反応ノート
読み込み中…