ethyl 2-(3-cyclopropylpyridin-2-yl)acetate synthesis

Yield:1214911-59-7 78%

Reaction Conditions:

with potassium phosphate;palladium diacetate;tricyclohexylphosphine in water;toluene at 100; for 24 h;

Steps:

31A

Example 31A A Schlenk tube was charged with 244 mg (1 mmol) of Example 12AA, 192.37 mg (1.3 mmol) of potassium cyclopropyltrifluoroborate, 742.93 mg (3.5 mmol) of tri-potassium phosphate, 11.23 mg (0.05 mmol) of palladium(II)acetate, 28.04 mg (0.1 mmol) of tricyclohexylphosphine in toluene (4 ml) and water (200 μl) and heated to 100° C. for 24 hours. After cooling a solid was filtered and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography on SiO₂ using n-hexane/ethyl acetate mixture of increasing polarity (from 100% n-hexane to 100% ethyl acetate) as eluant. 160 mg (78%) of the title compound were obtained.GC-MS (Method 3A): R_t: 11.08 minMS: 205 [M]⁺.

References:

US2012/115863,2012,A1 Location in patent:Page/Page column 52-53