反应详情

温度

160 °C

In a round-bottom flask fitted with reflux condenser and a drying tube filled with calcium chloride, 500 mg (1.70 mmol) of ethyl[2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate and 310 mg (1.70 mmol) of 1-(1-methylethyl)piperidin-4-carbohydrazide (Example 38A) were dissolved in 2 ml of 1-methyl-2-pyrrolidone, and the reaction mixture was stirred at 160° C. for 3 h. The reaction solution was cooled to 100° C., water (20 ml) was added and the mixture was then cooled to RT and stirred for 15 min. The reaction mixture was extracted with dichloromethane (3×50 ml), and the combined organic phases were dried over magnesium sulfate and concentrated. The crude product was chromatographed on basic aluminum oxide (mobile phase dichloromethane/methanol 10:1, then dichloromethane/methanol/17% strength aqueous ammonia solution 15:2:0.2). This gave 2.55 g (78% of theory) of the product.

1. customIn a round-bottom flask fitted
2. temperaturewith reflux condenser and a drying tube
3. temperatureThe reaction solution was cooled to 100° C.
4. temperaturethe mixture was then cooled to RT
5. stirringstirred for 15 min
6. extractionThe reaction mixture was extracted with dichloromethane (3×50 ml)
7. dry with materialthe combined organic phases were dried over magnesium sulfate
8. concentrationconcentrated
9. customThe crude product was chromatographed on basic aluminum oxide (mobile phase dichloromethane/methanol 10:1