反应详情

温度

-100 °C

A solution of LiHMDS in THF (77 mmol) is added to a mixture of 4-bromo-2,6-dimethylbenzenethiol (70 mmol) in THF (100 ml) at −78° C. over 15 minutes and the mixture stirred for an additional 2 hours. The mixture is cooled with liquid nitrogen to around −100° C. and a solution of 2,6-dichloro-4-methyl-5-nitropyrimidine (84 mmol) in THF (50 ml) is added rapidly. The reaction is maintained at around −100° C. for 1 hour and then allowed to warm to room temperature. The mixture is filtered and the isolated solid washed with ethanol. The filtrate may be concentrated and crystallized to obtain additional compound.

1. temperatureThe reaction is maintained at around −100° C. for 1 hour
2. temperatureto warm to room temperature
3. filtrationThe mixture is filtered
4. washthe isolated solid washed with ethanol
5. concentrationThe filtrate may be concentrated
6. customcrystallized
7. customto obtain additional compound