反应详情

温度

70 °C

(Step 4) To a suspension of 2-cyano-2-(3,4-dichloro-5-oxo-2,5-dihydrofuran-2-yl)acetamide (0.28 g) and 1-[5-chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride obtained in Step 3 (0.26 g) in ethanol (3 ml) was added N,N-diisopropylethylamine (0.44 ml) at room temperature, and the resulting mixture was heated under reflux for 4 hr. The reaction mixture was treated with water and stirred at 70° C. for 1 hr. After cooling to room temperature, the precipitate was collected by filtration and dried. The precipitate was suspended in methanol, and treated with a 2 M hydrogen chloride-methanol solution (0.3 ml). The resulting mixture was stirred at room temperature overnight. The precipitate was collected by filtration and dried to give the title compound (0.22 g) as white crystals.

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 4 hr
3. temperatureAfter cooling to room temperature
4. filtrationthe precipitate was collected by filtration
5. customdried
6. additiontreated with a 2 M hydrogen chloride-methanol solution (0.3 ml)
7. stirringThe resulting mixture was stirred at room temperature overnight
8. filtrationThe precipitate was collected by filtration
9. customdried