Ammonium Hydroxide → HCID 178516505、化合物
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1O[CH:5]=[CH:6][C:7](=[O:9])[CH:8]=1.[OH-].[NH4+:13]>CO>[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[C:7]([OH:9])[CH:6]=[CH:5][N:13]=1参加物
4
反応条件
- 温度
- 90 °C
実験手順
To a solution of 2-(trifluoromethyl)-4H-pyran-4-one (350 mg, 2.13 mmol) in MeOH (15 mL) was added ammonium hydroxide (14.8 mL, 107 mmol) at 25° C. The reaction mixture was stirred at 90° C. for 10 h, then concentrated, diluted with water and extracted with ethyl acetate. Combined organic portions were dried over Na2SO4, filtered and concentrated. Purification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3, CH3CN/water, 10˜95%, 9.5 min, 30 mL/min) afforded the title product (280 mg) as a yellow solid.
後処理
- concentrationconcentrated
- additiondiluted with water
- extractionextracted with ethyl acetate
- dry with materialCombined organic portions were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customPurification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3, CH3CN/water, 10˜95%, 9.5 min, 30 mL/min)
出典と根拠
- ORDレコード
- ord-d71d680a9d9f4ca1a7ffe91a9a396b90
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08975400B2
反応ノート
読み込み中…