反应详情

温度

100 °C

To 4,5-dichloro-1,2-phenylenediamine (25 g) was added 3,3,3-trifluoropropionic acid (25 mls) and 4N HCl (90 mL). The resulting mixture was heated to 100° C. overnight. The reaction mixture was quenched with water, basicified with concentrated NH4OH, extracted with EtOAc, and dried over Na2SO4. The crude product was filtered through a plug of silica gel, eluting with 30% EtOAc/hexanes, and collecting the red band. The fractions were concentrated to yield a mixture of the desired title compound and 4,5-dichloro-1,2-phenylenediamine. The crude material was dissolved in small amount of CH2Cl2 and triturated with hexanes to yield the title compound as a tan solid.

1. customThe reaction mixture was quenched with water
2. extractionextracted with EtOAc
3. dry with materialdried over Na2SO4
4. filtrationThe crude product was filtered through a plug of silica gel
5. washeluting with 30% EtOAc/hexanes
6. customcollecting the red band
7. concentrationThe fractions were concentrated
8. customto yield