Reacción #305162

Ecuación de reacción

2-methylpyrazine-5-carboxylic acid

tert-butyl 2,2,2-trichloroacetimidate

sodium chloride

ethyl acetate

→

title compound

Rendimiento 99.6%

t-butyl 5-methylpyrazine-2-carboxylate

Rendimiento 99.6%

Disolventes

tetrahydrofuran

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturacooling
2. 2
   Otrothe organic layer was separated
3. 3
   SecadoThe organic layer was dried over anhydrous magnesium sulfate
4. 4
   Otrothe insoluble matter was separated by filtration
5. 5
   ConcentraciónThe filtrate was concentrated
6. 6
   Otropurified by silica gel column chromatography

Procedimiento

A boron trifluoride-diethyl ether complex (91.7 IL) was added dropwise to a suspension of 2-methylpyrazine-5-carboxylic acid (1 g) and tert-butyl 2,2,2-trichloroacetimidate (4.75 g) in tetrahydrofuran (20 mL) under ice-cooling. The reaction solution was heated to room temperature and stirred for two hours. A saturated sodium chloride solution and ethyl acetate were added to the reaction solution, and the organic layer was separated. The organic layer was dried over anhydrous magnesium sulfate, and the insoluble matter was separated by filtration. The filtrate was concentrated and purified by silica gel column chromatography to obtain the title compound (1.4 g).

Fuente