反应详情

温度

100 °C

To a solution of 3.0 g (20 mmol) of 2,4-dichloro-pyrimidine in a 10:1 mixture of dioxane:water (220 mL) is added 3.3 g (22 mmol) of 2-hydroxy-3-methyl-phenyl boronic acid followed by 6.0 g (57 mmol) of sodium carbonate. Argon is bubbled through the solution for 15 min then 2.4 g (2.1 mmol) of tetrakis(triphenylphosphine)palladium (0) is added. The reaction is heated overnight at 100° C. then cooled to ambient temperature and filtered through diatomaceous earth. The filter pad is washed with EtOAc then placed on a new receiving flask and washed with a 1:1 mixture of MeOH:DCM. The filtrate is concentrated under reduced pressure to B-16 (1.60 g, 36.0%)

1. customArgon is bubbled through the solution for 15 min
2. temperaturethen cooled to ambient temperature
3. filtrationfiltered through diatomaceous earth
4. washThe filter pad is washed with EtOAc
5. washwashed with a 1:1 mixture of MeOH
6. concentrationThe filtrate is concentrated under reduced pressure to B-16 (1.60 g, 36.0%)