Reacción #367656

Ecuación de reacción

hydrocloride

sodium hydride

2-amino-4-cyclopropyl-6-methylpyrimidine

dimethylcarbonate

→

Methyl(4-cyclopropyl-6-methylpyrimidin-2-yl)carbamate

Disolventes

tetrahydrofuran

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONis added portionwise, under a nitrogen atmosphere
2. 2
   workup.STIRRINGThe suspension is stirred about 16 hours at ambient temperatures
3. 3
   Temperaturawhile maintaining a reaction temperature of 20° to 25° with external ice-bath
4. 4
   Temperaturacooling
5. 5
   workup.STIRRINGThe suspension is stirred 0.5 hour
6. 6
   Filtraciónfiltered
7. 7
   Secadothe filtrate is dried over sodium sulfate
8. 8
   Concentraciónconcentrated in vacuo
9. 9
   Otroto give the subject compound

Procedimiento

To a suspension of 53.7 g of 2-amino-4-cyclopropyl-6-methylpyrimidine in 1000 ml of tetrahydrofuran is added portionwise, under a nitrogen atmosphere, 42.8 g of 50% sodium hydride while cooling the reaction flask in an ice-water bath. After stirring one hour at 25° C. 58.5 g of dimethylcarbonate is added dropwise at 5° to 25°. The suspension is stirred about 16 hours at ambient temperatures, then 80 ml of concentrated hydrocloride acid is added dropwise under a nitrogen atmosphere while maintaining a reaction temperature of 20° to 25° with external ice-bath cooling. The suspension is stirred 0.5 hour, filtered, and the filtrate is dried over sodium sulfate and concentrated in vacuo to give the subject compound.

Fuente