反应详情

温度

3 °C

70% Perchloric acid (18.9 ml) was added to a 1,4-dioxane (26 ml) solution of (Z)-ethyl N-(mesitylsulfonyl)oxyacetimidate (11.7 g) at 4° C. over 20 minutes. Thereafter, the reaction solution was stirred at 3° C. for 30 minutes, and it was then poured into water (100 ml). The precipitated solid was collected by filtration, and was then washed with water (45 ml) to obtain a white solid as a crude product. Methyl 2-aminoisonicotinate (5 g) was added to methylene chloride (35 ml), and the obtained mixture was then cooled to 3° C. The obtained crude product was dissolved in methylene chloride (40 ml), and only an organic layer was added to a methylene chloride solution of 2-aminoisonicotinate. The obtained mixture was stirred at 3° C. for 30 minutes. Thereafter, methyl tert-butyl ether (50 ml) was added to the reaction solution, and the precipitated solid was collected by filtration. The collected solid was washed with methyl tert-butyl ether (20 nil), and was then dried at 45° C., so as to obtain the title compound (10.7 g) in the form of a light yellow solid.

1. filtrationThe precipitated solid was collected by filtration
2. washwas then washed with water (45 ml)
3. customto obtain a white solid as a crude product
4. temperaturethe obtained mixture was then cooled to 3° C
5. customThe obtained crude product
6. stirringThe obtained mixture was stirred at 3° C. for 30 minutes
7. filtrationthe precipitated solid was collected by filtration
8. washThe collected solid was washed with methyl tert-butyl ether (20 nil)
9. customwas then dried at 45° C.