反应详情

温度

0 °C

Dissolve 3-nitro-5-(trifluoromethyl)aniline (150 mg, 0.73 mmol), triethylamine (220 mg, 2.18 mmol) in DCM (8 mL), cool to 0° C. at ice bath, add slowly acryloyl chloride (198 mg, 2.18 mmol). After addition, stir the reaction at room temperature for 2 hrs. Pour the mixture into water (30 mL), extract with EtOAc (10 mL×3), combine the organic layers; wash with brine (50 mL), dry over anhydrous Na2SO4. Concentrate under reduced pressure to give the crude product (190 mg) which is used without further purification.

1. additionAfter addition
2. customthe reaction at room temperature for 2 hrs
3. extractionextract with EtOAc (10 mL×3)
4. washwash with brine (50 mL)
5. dry with materialdry over anhydrous Na2SO4
6. concentrationConcentrate under reduced pressure