Lithium hydroxide, monohydrate → 2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]acetic acid
反応式
O.[OH-].[Li+].C([O:6][C:7](=[O:18])[CH2:8][N:9]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[N:10]1)C>O.C1COCC1>[F:17][C:14]([F:15])([F:16])[C:11]1[CH:12]=[CH:13][N:9]([CH2:8][C:7]([OH:18])=[O:6])[N:10]=1参加物
5
実験手順
Lithium hydroxide monohydrate (127 mg, 3.03 mmol) in water (0.5 mL) was added to (3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid ethyl ester (250 mg, 1.125 mmol) in THF (5 mL). The mixture was stirred at room temperature for 5 hours then the reaction mixture volume was reduced to one third by evaporation in vacuo. The aqueous residue was acidified using aqueous HCl (2M) to pH=5. The resulting off white solid was filtered, collected and dried, washed with ether to afford the title compound as a white solid (42 mg, 19%).
後処理
- customthe reaction mixture volume was reduced to one third by evaporation in vacuo
- filtrationThe resulting off white solid was filtered
- customcollected
- customdried
- washwashed with ether
出典と根拠
- ORDレコード
- ord-9d52e78fb76b4841946e366f86da170a
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09163021B2
反応ノート
読み込み中…