反应详情

A solution of 4-(ethylamino)-2-methoxy-5-nitropyridine (5.0 g, 25.3 mmol) in POCl3 (25 mL) was heated to 100° C. in a sealed tube for 1 week. The reaction mixture was cooled and concentrated and the residue was taken up in EtOAc/H2O and carefully quenched with sat. K2CO3. The aqueous layer was extracted with EtOAc, washed with H2O, dried (MgSO4) and concentrated to give an orange oil which solidified on standing which was used without further purification. MS (ES+) m/e 202 [M+H]+.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated
3. customcarefully quenched with sat. K2CO3
4. extractionThe aqueous layer was extracted with EtOAc
5. washwashed with H2O
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customto give an orange oil which
9. customwas used without further purification