反应详情

3-(Hydroxymethyl)-2-(1-hydroxypropan-2-yl)-3,4-dihydroisoquinolin-1(2H)-one (from Isomer B, 0.20 g, 0.85 mmol) in chloroform (7.6 ml) was added to a stirring solution of thionyl chloride (1.8 ml) in chloroform (10 ml). After refluxing overnight the condenser was removed and the majority of the solvent allowed to evaporate over the next 4 h. The residue was purified by flash chromatography (SiO2, CH2Cl2 to 50% EtOAc in CH2Cl2) affording pure product (0.16 g, 69% yield). MS (ESI) 273/275 (M+H).

1. temperatureAfter refluxing overnight the condenser
2. customwas removed
3. customto evaporate over the next 4 h
4. customThe residue was purified by flash chromatography (SiO2, CH2Cl2 to 50% EtOAc in CH2Cl2)