反应详情

To a stirred, refluxing mixture of 5.00 g of 2,3-dichloroquinoxaline in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 14.00 g of methyl diphenylphosphinite. The mixture was refluxed for 6 hours after the addition was completed and then allowed to stand overnight at room temperature. The next day the mixture was admixed with 500 ml of n-hexane, and the resulting solid was separated by filtration, washed with hexane, recrystallized from 100 ml of chlorobenzene, and dried at 100° C./0.1 mm (13 Pa) to give 9.87 g of 2,3-bis(diphenylphosphinyl)-quinoxaline (shown by formula in Claim 6) as a very slightly yellowish-white solid, mp 258°-272° C. with decomposition. Anal. Calcd for C32H24N2O2P2 : C, 72.45; H, 4.56; N, 5.28; P, 11.68. Found: C, 72.38; H, 4.23; N, 5.18; P, 11.39.

1. temperatureTo a stirred, refluxing
2. temperatureThe mixture was refluxed for 6 hours
3. additionafter the addition
4. customthe resulting solid was separated by filtration
5. washwashed with hexane
6. customrecrystallized from 100 ml of chlorobenzene
7. customdried at 100° C./0.1 mm (13 Pa)