反应详情

10.1 g (45.6 mmol) of 3-(4-methyl-5-nitro-1,3-thiazol-2-yl)pyridine (for preparation see DE 2221647) were dissolved in 100 ml of 10% hydrochloric acid together with 10 ml of conc. hydrochloric acid, and 25 g of tin(II) chloride dissolved in 10% hydrochloric acid were added in portions, and the mixture was stirred for 1 h (hour), in the course of which heating occurred. The mixture was poured into ice/sodium hydroxide solution, methyl t-butyl ether, ethyl acetate and saturated sodium chloride solution were added, the mixture was extracted 4 times at pH=10 with ethyl acetate, the combined organic phases were dried with Mg504 and the mixture was concentrated. The residue was recrystallized from benzotrifluoride.

1. additionwere added in portions
2. temperaturein the course of which heating
3. additionwere added
4. extractionthe mixture was extracted 4 times at pH=10 with ethyl acetate
5. customthe combined organic phases were dried with Mg504
6. concentrationthe mixture was concentrated
7. customThe residue was recrystallized from benzotrifluoride