反应详情

温度

160 °C

To a solution of 8-bromo-2-[1,3,4]oxadiazol-2-yl-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene (4.38 g, 12.51 mmol) in pyridine (12 mL) was added isopropylamine hydrochloride (1.38 g, 12.51 mmol). The reaction mixture was heated at 160° C. for 30 minutes using microwave irradiation before being concentrated in vacuo. The residue was taken up into DCM then washed with 1M HCl then brine before being dried (Na2SO4) and concentrated in vacuo. The resultant residue was purified by flash chromatography (SiO2, gradient 0-3% methanol in DCM then further purified, gradient 0-4% MeOH in EtOAc) to yield the title compound as an orange solid (1.97 g, 40%). LCMS: RT=4.67 min, M+H+=391/393.

1. custommicrowave irradiation
2. concentrationbefore being concentrated in vacuo
3. washthen washed with 1M HCl
4. dry with materialbrine before being dried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customThe resultant residue was purified by flash chromatography (SiO2, gradient 0-3% methanol in DCM
7. customthen further purified