反应详情

To a solution of 4-chloro-3-nitroaniline (1.72 g, 10.0 mmol) in 60 mL of anhydrous DCM was added crystalline DMAP (1.22 g, 10.0 mmol). The reaction mixture was stirred until all solids dissolved, then 3-trifluoromethylbenzoyl chloride (2.71 g, 13.0 mmol) was added dropwise. The reaction mixture was left to stir at ambient temperature for 6 hrs. The completion of the reaction was monitored by TLC and LC/MS. Then it was transferred into a separatory funnel and washed with water (3×100 mL), saturated NaHCO3 (2×100 mL), brine (1×100 mL), dried over anhydrous Na2SO4 and filtered through a short pad of silica gel. Solvent was removed in vacuo to give the title product as a light-brown solid (3.4 g, 100% yield).

1. dissolutiondissolved
2. waitThe reaction mixture was left
3. stirringto stir at ambient temperature for 6 hrs
4. customThen it was transferred into a separatory funnel
5. washwashed with water (3×100 mL), saturated NaHCO3 (2×100 mL), brine (1×100 mL)
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered through a short pad of silica gel
8. customSolvent was removed in vacuo