反应详情

温度

120 °C

1,4-dichlorophthalazine (5.00 g, 25.1 mmol) and (R)-tert-butyl 3-methylpiperazine-1-carboxylate (11.06 g, 55.2 mmol) were mixed intimately and placed in a flask under an Argon atmosphere. The flask was heated at 120° C. for approximately 16 hours, after which time LC/MS showed disappearance of the starting material. The reaction was cooled, taken up in dichloromethane (150 mL), and washed once with aqueous sodium bicarbonate (50% of saturated) and once with saturated sodium chloride solution. The organic phase was dried (MgSO4) and evaporated to give an orange oil. Chromatography over silica gel with a gradient of hexanes/0-10% acetone gave a pale yellow solid JK-1. MS (M+H)+=363.1.

1. customplaced in a flask under an Argon atmosphere
2. temperatureThe reaction was cooled
3. washwashed once with aqueous sodium bicarbonate (50% of saturated) and once with saturated sodium chloride solution
4. dry with materialThe organic phase was dried (MgSO4)
5. customevaporated
6. customto give an orange oil