反应详情

A suspension of 100 parts of 6-chloro-2,3-diaminoquinoxaline in 1000 parts of pyridine was cooled to 5° in an ice bath. A solution of 152 parts of valeryl chloride in 130 parts of tetrahydrofuran was added quickly with good cooling to prevent the temperature from rising above 20°. The reaction mixture was stirred at ambient temperature for 1 hour and then poured into 2500 parts of water. The solid which separated was removed by filtration and washed with water, methanol, and then ether. The crude product was recrystallized from methanol to yield 55 parts of 6-chloro-2,3-bis-(valeramido)quinoxaline, m.p. 171°-173°, as a colorless solid.

1. temperaturewas cooled to 5° in an ice bath
2. temperaturewith good cooling
3. customfrom rising above 20°
4. customThe solid which separated
5. customwas removed by filtration
6. washwashed with water, methanol
7. customThe crude product was recrystallized from methanol