反応 #249
ord-dfcce3a0a05b417eb954f008fad9e74c
溶媒
反応条件
実験手順
TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (1.238 g, 1.35 mmol) was added in one portion to 2,4-dichloropyridine (10g, 67.57 mmol), 1-methyl-1H-pyrazol-5-amine (7.22 g, 74.33 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (2.346 g, 4.05 mmol) and sodium tert-butoxide (9.74 g, 101.36 mmol) in 1,4-dioxane (500 mL) warmed to 130ºC over a period of 10 minutes under nitrogen. The resulting mixture was stirred at 130 °C for 24 hours. The reaction mixture was evaporated to dryness and redissolved in DCM (300 mL), and washed with water (125 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 4% MeOH in DCM. Pure fractions were evaporated to dryness to afford EN01861-14-01 (2.93 g, 20.8 %) as a yellow crystalline solid. EN01861-14-01 (2.93 g) was combined with EN01861-09-01 (2.63g) to give EN01861-14-02 (5.56 g) as a yellow crystalline solid.