反应详情

To a solution of 5-chloro-1,3-phenylenediamine (2.00 g) in acetic acid (20 mL) was added 2,5-dimethoxytetrahydrofuran (1.8 mL). After 4 hours at reflux, the reaction mixture was concentrated. The residue was suspended in satd. NaHCO3 and EtOAc. The reaction mixture was filtered and the organic layer was collected, washed with satd. NaHCO3 and brine, dried (Na2SO4), filtered and concentrated. Purification of the residue by chromatography (silica gel: EtOAc/hexane: 1/4) afforded 0.54 g of 3-chloro-5-(l-pyrrolyl) aniline. MS (m/z) 193 (MH+).

1. temperatureAfter 4 hours at reflux
2. concentrationthe reaction mixture was concentrated
3. filtrationThe reaction mixture was filtered
4. customthe organic layer was collected
5. washwashed with satd
6. dry with materialNaHCO3 and brine, dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification of the residue by chromatography (silica gel: EtOAc/hexane: 1/4)