反应详情

To a solution of 3-(diethylamino)phenol (0.0104 g, 0.631 mmol) in acetonitrile (4 mL) was added 1,3-dibromopropane (0.640 mL, 6.30 mmol) followed by Cs2CO3 (0.313 g, 0.961 mmol). The reaction mixture was stirred for 24 h and then concentrated under vacuum. The resulting residue was treated with H2O (4 mL) and extracted with DCM (8 mL). The organic layer was dried through a phase separator and concentrated under vacuum. The residue was taken up in DMSO and purified by preparatory HPLC (without TFA) to give the title compound (0.0314 g, 17.4%). EI-MS m/z 286(M+H+) Rt (1.59 min).

1. concentrationconcentrated under vacuum
2. additionThe resulting residue was treated with H2O (4 mL)
3. extractionextracted with DCM (8 mL)
4. customThe organic layer was dried through a phase separator
5. concentrationconcentrated under vacuum
6. custompurified by preparatory HPLC (without TFA)