反应详情

Dissolve [4-(2-azepan-1-yl-ethoxy)-phenyl]-[6-hydroxy-2-(2,3,5-trifluoro-phenyl)-naphthalen-1-yl]-methanone (2.63 g, 5.1 mmol) in 60 mL dioxane and add 10 mL of a 1.0 M solution of lithium triethylborohydride in THF. At the end of one hour, add another 10 mL of the lithium reagent mixture is added and gently warm the reaction. After a further one hour, add an additional 25 ml of lithium triethylborohydride and heat the reaction to reflux and hold for 8 hours. Cool the reaction and quench with water. Extract the water with methylene chloride, dry the organic layer with molecular sieves and concentrate. Purify on a silica gel column eluting with a 0-10% methanol/methylene chloride gradient.

1. additionis added
2. temperaturegently warm
3. customthe reaction
4. temperatureheat
5. customthe reaction
6. temperatureto reflux
7. waithold for 8 hours
8. temperatureCool
9. customthe reaction
10. customquench with water
11. extractionExtract the water with methylene chloride
12. customdry the organic layer with molecular sieves
13. concentrationconcentrate
14. customPurify on a silica gel column
15. washeluting with a 0-10% methanol/methylene chloride gradient