HRID1064085

反应详情

EQUATION

反应方程式

HRID 1064085 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a 100 mL round bottom flask, was added 0.1 g 4-(3,4-Dichloro-phenyl)-1-isopropyl-5-pyridin-4-yl-pyrazolidin-3-one and 10 mL THF, stirred at 0° C. under nitrogen. 0.43 mL 1 M LHMDS in THF was added drop wise. After stirred at 0° C. for 30 min 0.026 mL iodomethane was added drop wise. The resulted mixture was stirred from 0° C. to rt for 2 hours, quenched with 20 mL sat. NH4Cl, extracted with dichloromethane 3×25 mL. The organic phase was dried over anhydrous Na2SO4. After purification by flash chromatography, obtained the title compound 80 mg as light solid. MS (ES+): 364 (M+H)+.

WORKUP

后处理

  1. additionwas added drop wise
  2. stirringThe resulted mixture was stirred from 0° C. to rt for 2 hours
  3. customquenched with 20 mL sat. NH4Cl
  4. extractionextracted with dichloromethane 3×25 mL
  5. dry with materialThe organic phase was dried over anhydrous Na2SO4
  6. customAfter purification by flash chromatography