反应详情

NaH (5.30 g, 0.132 mol) was added in portions to a solution of 5-chloro-6-nitroisoindoline-1,3-dione (20.0 g, 88.27 mmol) in 100 mL of anhydrous DMF at 0° C. under argon. The reaction mixture was then stirred at rt for 3 h. 2-Iodopropane (15.0 g, 106 mol) was added dropwise via a syringe at rt under argon. The resulted mixture was stirred for 6 h at rt, hydrolyzed by adding 200 mL of water. The precipitate was isolated, washed with water and dried under vacuum. The solid was purified by column chromatography (silica-gel, CH2Cl2/Acetone=19/1 v/v) to give a solid product.

1. stirringThe resulted mixture was stirred for 6 h at rt
2. customThe precipitate was isolated
3. washwashed with water
4. customdried under vacuum
5. customThe solid was purified by column chromatography (silica-gel, CH2Cl2/Acetone=19/1 v/v)
6. customto give a solid product