Реакция #1135851
ord-c793924ab4d740a896acec8a0791da6e
Уравнение реакции
Реагенты
Нет
Условия реакции
Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Промывкаwashed with water
- 2ЭкстракцияThe organic extract
- 3Другоеwas dried
- 4Концентрированиеconcentrated
- 5Другоеpurified by column chromatography
Методика
3-Amino-5-bromo pyridine (XVIII) (1 eq) was dissolved in DCM and cooled to 0° C. before adding pyridine (2.2 eq) and isobutyryl chloride (XIX) (1.1 eq). The reaction mixture was stirred at r.t. for 15 h until TLC showed the reaction was complete. The reaction mixture was diluted with DCM and washed with water. The organic extract was dried, concentrated and purified by column chromatography using silica gel (100-200 mesh) to afford N-(5-bromopyridin-3-yl)isobutyramide (XX) as a off white solid, (71% yield). 1H NMR (CDCl3) δ ppm 8.55-8.35 (m, 3H), 7.32 (s, 1H), 2.59-2.48 (m, 1H), 1.28-1.27 (d, 6H); ESIMS found C9H11BrN2O m/z 243.05 (M+H).