反应详情

To a suspension 2-hydrazinyl-3-methyl-5-nitropyridine (Step 67.1) (33.2 g, 198 mmol) in dioxane (175 mL) was added Ac2O (20.5 mL, 217 mmol) and the reaction was stirred at RT for min. The reaction mixture was poured onto ice-water and stirred for 1 hr at 0° C. The precipitate was collected by filtration, washed with H2O and Et2O, and dried under reduced pressure at 50° C. to afford the title product (41.5 g, 198 mmol, 99.5% yield) as light beige solid. tR: 0.45 min (LC-MS 2); ESI-MS: 211 [M+H]+; ESI-MS: 209 [M−H]− (LC-MS 2).

1. additionThe reaction mixture was poured onto ice-water
2. stirringstirred for 1 hr at 0° C
3. filtrationThe precipitate was collected by filtration
4. washwashed with H2O and Et2O
5. customdried under reduced pressure at 50° C.