Water → Acetic acid 3,5-dichloro-4'-(4-trifluoromethyl-piperidine-1-carbonyl)-biphenyl-4-ylmethyl Ester

温度

80 °C

Dissolve 18.5 g (1 eq.) of Acetic acid 2,6-dichloro-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzyl ester and 19.9 g (1.1 eq.) of (4-Bromo-phenyl)-(4-trifluoromethyl-piperidin-1-yl)-methanone in 190 mL of dimethoxyethane. Add 8.9 g of potassium carbonate, 95 mL of water, 0.24 g (0.02 eq.) of palladium acetate and 0.85 g (0.06 eq.) of triphenylphosphine. Heat the mixture at 80° C. for 2.5 hours. Stir the reaction mixture at room temperature overnight to afford a suspension. Add 7.4 g of potassium carbonate, 100 mL of water and 100 mL of methanol and stir the mixture at room temperature for 3 hours. Collect the solid by filtration and dry in a vacuum oven at 50° C. to afford 20.8 g (82% yield) of the titled compound.

1. customto afford a suspension
2. stirringstir the mixture at room temperature for 3 hours
3. customCollect the solid
4. filtrationby filtration
5. customdry in a vacuum oven at 50° C.

ORDレコード

ord-1147736152ca4270ac128776b5ee98a2

出典データセット

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08153807B2