反应详情

温度

0 °C

Dissolve [6-hydroxy-2-(2,4,6-trifluoro-phenyl)-naphthalen 1-yl]-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methanone (728 mg, 1.4 mmol) in THF (85 mL) and cool to 0° C. Add 1M lithium aluminum hydride in THF (5.8 mL, 5.8 mmol) and bring to room temperature. Heat the reaction to reflux for 30 minutes. Cool reaction and pour onto ice/chloroform to form a suspension. Add 6N HCl dropwise to obtain a pH of 1. Extract with 20% isopropyl alcohol in chloroform. Wash organic layer with brine, dry, filter, and concentrate in vacuo to yield 730 mg (100%) of the title compound. HPLC Rt (0.01% heptafluorobutyric acid:1.0% isopropylalcohol:water is mobile phase A and 0.01% heptafluorobutyric acid:1.0% isopropylalcohol:acetonitrile is mobile phase B; gradient: 5 to 95% B, Purity@254 nm)=2.41 (100%); mass spectrum (ion spray): m/z=508.3 (M+H).

1. custombring to room temperature
2. temperatureHeat
3. customthe reaction
4. temperatureto reflux for 30 minutes
5. temperatureCool
6. customreaction
7. additionpour onto ice/chloroform
8. customto form a suspension
9. customto obtain a pH of 1
10. extractionExtract with 20% isopropyl alcohol in chloroform
11. dry with materialWash organic layer with brine, dry
12. filtrationfilter
13. concentrationconcentrate in vacuo