HRID1484814

反应详情

EQUATION

反应方程式

HRID 1484814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationthe mixture was concentrated
  2. additionwas diluted with Sat. NaHCO3 and EtOAc, organic layer
  3. customwas separated
  4. extractionthe aqueous layer was extracted with EtOAc, organic layer ere
  5. washwashed with brine
  6. customdried
  7. concentrationconcentrated
  8. customto give crude oil, which
  9. customwas purified by column (Hexanes/EtOAc=100:0 to 25:75)