反应详情

温度

80 °C

To a single-necked 250 mL round-bottomed flask equipped with a magnetic stirrer and reflux condenser was charged (−)-1,4-dimethyl-3-(4-aminophenyl)piperazin-2-one (8.2 g, 37.3 mmol), 3,5-dibromo-1-methylpyrazin-2(1H)-one (10.0 g, 37.3 mmol), and i-PrOH (100 mL). Triethylamine (5.72 mL, 41 mmol, 1.1 eq) was then added and the resulting suspension was heated at 80° C. for 16 hrs. A thick slurry was observed the following day. The reaction was cooled to room temperature then concentrated in vacuo to ˜20 mL total volume. At that point 20 mL of 2M Na2CO3 solution was added followed by 100 mL of water. The mixture was then allowed to slurry for 2 hrs at room temperature. The off-white solid was then collected on a fritted funnel and allowed to air dry for ˜1 hr. The solids were returned to the reaction flask and 100 mL of diethyl ether/hexanes (1:1) was added and the suspension was triturated at room temperature for 1 hr. The white solid was then collected on a fritted funnel, dried on the filter with vacuum for 1 hr, then transferred to a round-bottomed flask and vacuum-dried overnight. White solids were obtained, 12.88 g (85%).

1. customTo a single-necked 250 mL round-bottomed flask equipped with a magnetic stirrer
2. temperaturereflux condenser
3. temperatureThe reaction was cooled to room temperature
4. concentrationthen concentrated in vacuo to ˜20 mL total volume
5. additionAt that point 20 mL of 2M Na2CO3 solution was added
6. customThe off-white solid was then collected on a fritted funnel
7. customto air dry for ˜1 hr
8. additionwas added
9. customthe suspension was triturated at room temperature for 1 hr
10. customThe white solid was then collected on a fritted funnel
11. customdried on the
12. filtrationfilter with vacuum for 1 hr
13. customtransferred to a round-bottomed flask
14. customvacuum-dried overnight
15. customWhite solids were obtained