反応 #62181

反応方程式

4-[3-(4-Benzyloxy-2-fluoro-phenyl)-1-(2,2,2-trifluoro-ethyl)-1H-pyrazol-4-yl]-pyridine

trifluoroacetic acid

anisole

→

title compound

収率 77.7%

3-Fluoro-4-[4-pyridin-4-yl-1-(2,2,2-trifluoro-ethyl)-1H-pyrazol-3-yl]-phenol

収率 77.7%

反応条件

後処理

1. 1
   温度the reaction mixture heated
2. 2
   温度at reflux for 18 h
3. 3
   その他The reaction mixture was quenched with with 1N NaOH
4. 4
   抽出extracted 3× tetrahydrofuran, dried magnesium sulfate
5. 5
   ろ過filtered
6. 6
   濃縮concentrated
7. 7
   その他Purification via Biotage MPLC
8. 8
   洗浄eluting with 5% methanol/1% ammonium hydroxide/ethyl acetate

実験手順

To 4-[3-(4-Benzyloxy-2-fluoro-phenyl)-1-(2,2,2-trifluoro-ethyl)-1H-pyrazol-4-yl]-pyridine (900 mg) was added trifluoroacetic acid (5.25 ml) and anisole (1.15 ml) and the reaction mixture heated at reflux for 18 h. The reaction mixture was quenched with with 1N NaOH, extracted 3× tetrahydrofuran, dried magnesium sulfate, filtered and concentrated. Purification via Biotage MPLC eluting with 5% methanol/1% ammonium hydroxide/ethyl acetate provided the title compound (552 mg). MS: (M+H m/z=338.2).

出典