反应详情

温度

150 °C

5-Chloro-2-isopropyl-6-nitroisoindoline-1,3-dione (14.40 g, 59.85 mmol) and urea (35.95 g, 599 mmol) were mixed together under argon. The mixture was stirred and heated to 150° C. for 3 h and cooled to rt. The solid was washed with 200 mL of hot water (90° C.) and filtered to remove the remaining urea. The isolated yellow solid was washed twice with hot water, dried under vacuum and purified by column chromatography (silica-gel CH2Cl2/acetone=19/1 v/v) to give a solid product.

1. temperaturecooled to rt
2. washThe solid was washed with 200 mL of hot water (90° C.)
3. filtrationfiltered
4. customto remove the remaining urea
5. washThe isolated yellow solid was washed twice with hot water
6. customdried under vacuum
7. custompurified by column chromatography (silica-gel CH2Cl2/acetone=19/1 v/v)
8. customto give a solid product