反应详情

温度

90 °C

A mixture of 3-chloro-6-hydrazinylpyridazine (200 g, 1.38 mol) and isobutyryl chloride (175 mL, 1.66 mol) in 1,4-dioxane (2 L) was heated at about 90° C. overnight. The suspension was cooled to about 5° C. in an ice bath and then water (2 L) was added followed by slow addition of Na2CO3 (275 g, 2.59 mol). The resulting solution was extracted with DCM (3×1 L). The combined organic extracts were dried over MgSO4, concentrated under reduced pressure, and dried under vacuum overnight to give the title compound (255 g, 94%): LC/MS (Table 1, Method a) Rt=2.04 min; MS m/z: 197.1 (M+H)+.

1. temperatureThe suspension was cooled to about 5° C. in an ice bath
2. extractionThe resulting solution was extracted with DCM (3×1 L)
3. dry with materialThe combined organic extracts were dried over MgSO4
4. concentrationconcentrated under reduced pressure
5. customdried under vacuum overnight