HRID1484814
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 1-(4-(hydroxymethyl)-3-phenyl-5,6-dihydropyridin-1(2H)-yl)ethanone (86 mg, 0.37 mmol) in DCM (2 mL) was added SOCl2 (0.67 mL, 9.25 mmol). After stirred at RT for 15 min, the mixture was concentrated and was diluted with Sat. NaHCO3 and EtOAc, organic layer was separated and the aqueous layer was extracted with EtOAc, organic layer ere combined, washed with brine, dried and concentrated to give crude oil, which was purified by column (Hexanes/EtOAc=100:0 to 25:75) to give 1-(4-(chloromethyl)-5-phenyl-3,6-dihydropyridin-1(2H)-yl)ethan-1-one (35 mg).
WORKUP
后处理
- concentrationthe mixture was concentrated
- additionwas diluted with Sat. NaHCO3 and EtOAc, organic layer
- customwas separated
- extractionthe aqueous layer was extracted with EtOAc, organic layer ere
- washwashed with brine
- customdried
- concentrationconcentrated
- customto give crude oil, which
- customwas purified by column (Hexanes/EtOAc=100:0 to 25:75)