反应详情

温度

100 °C

In a 5 mL round bottomed flask were mixed: 1,1-dimethylethyl 1-piperazinecarboxylate (110 mg, 0.590 mmol, available from Fluke), 2-bromo-5-iodopyrazine (140 mg, 0.491 mmol, available from Apollo) and Dipea (0.112 mL, 0.639 mmol) in Tert-Butanol (2 mL). The reaction was stirred and heated under reflux at 100° C. for 40 hr. The reaction mixture was partitioned between EtOAc (20 mL) and water (20 mL) and the organic layer washed with brine (20 mL) before being dried through an hydrophobic frit and concentrated. The samples were dissolved in 1:1 MeOH:DMSO 2×1 mL and purified by MDAP. The solvent was evaporated in vacuo to give the required product 1,1-dimethylethyl 4-(5-iodo-2-pyrazinyl)-1-piperazinecarboxylate (98.6 mg) LCMS (Method C): Rt=1.20, MH+=391

1. additionIn a 5 mL round bottomed flask were mixed
2. temperatureheated
3. customThe reaction mixture was partitioned between EtOAc (20 mL) and water (20 mL)
4. washthe organic layer washed with brine (20 mL)
5. custombefore being dried through an hydrophobic frit
6. concentrationconcentrated
7. dissolutionThe samples were dissolved in 1:1 MeOH
8. customDMSO 2×1 mL and purified by MDAP
9. customThe solvent was evaporated in vacuo