反应详情

tert-butyl N-[[4-[[(3-amino-6-bromo-pyrazine-2-carbonyl)amino]carbamoyl]phenyl]methyl]-N-methyl-carbamate (7.66 g, 15.98 mmol) was dissolved in dry acetonitrile (114.9 mL) and cooled in an ice bath and put under a nitrogen atmosphere. Diisopropylethylamine (6.196 g. 8.350 mL, 47.94 mmol) was added via a syringe followed by dibromo(triphenyl)phosphorane (8.767 g, 20.77 mmol) portion wise. Reaction mixture started to precipitate out therefore left to stir for 45 minutes in an ice bath and isolated precipitated product by filtration as a beige powder (4.5 g). This material was then sonicated, triturated in acetonitrile, filtered and dried to give the sub-titled compound as yellow solid. (3.17 g, 40.9%). 1H NMR (400 MHz, DMSO-d6) δ 1.38-1.45 (br d, 9H), 2.80 (s, 3H), 4.45 (s, 2H), 7.48-7.51 (br s, 2H), 7.80 (br s, 2H), 8.10-8.20 (m, 2H), 8.45 (s, 1H) ppm; LC/MS m/z 463.1, 464.2 [M+H]+.

1. temperaturecooled in an ice bath
2. customReaction mixture
3. customto precipitate
4. waitout therefore left
5. customisolated
6. customprecipitated product
7. filtrationby filtration as a beige powder (4.5 g)
8. customThis material was then sonicated
9. customtriturated in acetonitrile
10. filtrationfiltered
11. customdried