Réaction #612
ord-fde5e0f95519439ca9660af435fc14a6
Équation de réaction
Cc1cnc(Cl)c(F)c1
CC(C)(C)OC(N)=O
→
Cc1cnc(NC(=O)OC(C)(C
Rendement 25.7%
Réactifs
Solvants
Conditions de réaction
Température
100°CELSIUS
Mode opératoire
diacetoxypalladium (15.42 mg, 0.07 mmol) and(9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (39.8 mg, 0.07 mmol) were added to a degassed mixture of 2-chloro-3-fluoro-5-methylpyridine (100 mg, 0.69 mmol), tert-butyl carbamate (105 mg, 0.89 mmol) and 2-chloro-3-fluoro-5-methylpyridine (100 mg, 0.69 mmol) in dioxane (10 mL) at 21°C. The resulting mixture was stirred at 100 °C for 2 hours.Cooled. Adsorbed onto silica. The crude product was purified by flash silica chromatography, elution gradient 10 to 30% DCM in heptane. Pure fractions were evaporated to dryness to afford tert-butyl 3-fluoro-5-methylpyridin-2-ylcarbamate (40.0 mg, 25.7 %) as a cream solid. not pure enough to register ..
Source
750 AstraZeneca ELN dataset