Chloroform → HCID 86607573, compound

Participants

Reaction Conditions

Reaction Steps

In a 10 ml reaction vessel were dissolved 55 mg (0.23 mmol) 3-Amino-6-methyl-pyridine-2-carboxylic acid (2-chloro-pyridin-4-yl)-amide (example 5) and 81 mg (0.45 mmol, 2.0 equiv.) of 3-Bromo-4-methylpyridine in 3 ml of dioxane. Cesium carbonate (148 mg, 0.45 mmol, 2.0 equiv.) were added and argon was bubbled through the suspension for 3 min. Then Xanthphos (43 mg, 0.075 mmol, 0.33 equiv.) and Pd2(dba)3.CHCl3 (23.5 mg, 0.023 mmol, 0.1 equiv.) were added, the vessel was closed and the mixture was heated for 19 h at 130° C. To the mixture was added silicagel (5 g) and the mixture was evaporated to dryness in vaccuo. The powder was charged onto a flash chromatography column and eluted (heptane/ethyl acetate 4:1) to yield the title compound as a yellow crystalline solid (total 28 mg, 28%), MS (ISP): m/e=334.0 (M+H+).

Provenance & Evidence