反应详情

10 g of 3-amino-5-t-butylpyrazole as prepared in Reference Example (this pyrazole compound being hereinafter referred to as "Compound [II]") was dissolved in 100 ml of carbon tetrachloride, and 6.8 g of methyl chloroformate was added to the solution. The mixture was then allowed to react for 5 hours under refluxing. After cooling the reaction solution, a potassium carbonate aqueous solution was added thereto whereby crystals were formed. The crystals were collected by filtration, and washed with carbon tetrachloride and water to obtain 3.8 g of methyl N-(5-t-butyl-3-pyrazolyl)carbamate. This compound was recrystallized from a mixed solvent of carbon tetrachloride and chloroform and found to have a melting point of 177° C.

1. customto react for 5 hours
2. temperatureunder refluxing
3. temperatureAfter cooling the reaction solution
4. customwhereby crystals were formed
5. filtrationThe crystals were collected by filtration
6. washwashed with carbon tetrachloride and water