反应详情

温度

100 °C

Dissolve trifluoromethanesulfonic acid 6-methoxy-1-[4-(2-piperidin-1-yl-ethoxy)-phenoxy]-naphthalen-2-yl ester (1.0 gm., 1.9 mmoles) in 20 ml DMF. To this solution add 2,6-difluorophenylboronic acid (0.6 gm., 3.8 mmoles), potassium phosphate (2.42 gm., 11.4 mmoles) and tetrakis(triphenylphosphine)palladium (0) (0.44 gm., 0.38 mmoles) and heat to 100° C. for 18 hours. Cool and filter the mixture and purify on an SCX column, eluting the impurities with methanol, then eluting the product with 2N ammonia/methanol. Purify further on a silica gel column eluting with a gradient of 50-100% methylene chloride/hexane containing 1% isopropyl amine to give 300 mg (32%) of the title compound.

1. temperatureCool
2. filtrationfilter the mixture
3. custompurify on an SCX column
4. washeluting the impurities with methanol
5. washeluting the product with 2N ammonia/methanol
6. customPurify further on a silica gel column
7. washeluting with a gradient of 50-100% methylene chloride/hexane containing 1% isopropyl amine