反应详情

2-Chloro-pyridin-4-ylamine (1 eq, 6.6 mmol, 850 mg) and 2,6-dibromo-3-nitro pyridine (2 eq, 13.2 mmol, 3.85 g) are dissolved in IPA (15 ml) and heated using microwave radiation at 150° C. for 6 hours. After cooling to room temperature, triethylamine (1 eq) is added and reaction mixture is stirred for 1 hour. The majority of solvent is removed in vacuo and the residue is diluted using 6% DCM in iso-hexane (75 ml). The solvent is decanted off and the process repeated 3 times. The resulting brown solid is dissolved in DCM and excess amine is scavenged using SCX-2 resin (6 g) and discarded. The solid is triturated in hexane, DCM and IPA (50 ml of a 58:40:2 mixture) and the resulting yellow solid is collected by filtration. The solid is dissolved in DCM and washed with water. The organic portion is dried (MgSO4) and concentrated in vacuo to afford the title compound; [M+H]+ 330.

1. temperatureheated
2. customat 150° C.
3. customfor 6 hours
4. customreaction mixture
5. customThe majority of solvent is removed in vacuo
6. additionthe residue is diluted
7. customThe solvent is decanted off
8. dissolutionThe resulting brown solid is dissolved in DCM
9. customThe solid is triturated in hexane
10. filtrationDCM and IPA (50 ml of a 58:40:2 mixture) and the resulting yellow solid is collected by filtration
11. dissolutionThe solid is dissolved in DCM
12. washwashed with water
13. dry with materialThe organic portion is dried (MgSO4)
14. concentrationconcentrated in vacuo