反应详情

To a vigorously stirring suspension of NaN3 (55 g, 0.85 mol) in 1:1; dioxane:H2O (200 mL) cooled to 0° C. was added dropwise over 20 min a solution of 3-cyano-3-thiophen-2-yl-acryloyl chloride 22 (84.3 g, 0.428 mol) in dioxane (150 mL). After stirring at 0° C. for 20 min, the reaction was warmed to room temperature and stirred for 1 h. To the reaction solution was added 600 mL H2O, thus producing a precipitate which was filtered, washed with H2O and dried under vacuum to provide pure 85 g of 23.

1. stirringAfter stirring at 0° C. for 20 min
2. stirringstirred for 1 h
3. customthus producing a precipitate which
4. filtrationwas filtered
5. washwashed with H2O
6. customdried under vacuum