反应详情

To a solution of 4-hydroxybenzonitrile (0.109 g, 0.913 mmol) in acetonitrile (4 mL) was added 1,3-dibromopropane (0.930 mL, 9.16 mmol) followed by Cs2CO3 (0.439 g, 1.35 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 (0.156 g, 71.4%). EI-MS Rt (2.10 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)