HRID2365979

反应详情

EQUATION

反应方程式

HRID 2365979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of methanesulfonic acid (R)-(7-fluoro-2,3-dihydrobenzo[1,4]dioxin-2-yl)methyl ester (51 mg, 0.19 mmol), (R*)-3-(piperidin-3-yl)phenol HBr (50 mg, 0.19 mmol) and NaHCO3 (33 mg, 0.39 mmol) in DMF (3.5 ml) was heated at 120° C. for 1.5 h. Water (10 ml) was added to the cooled mixture, which was then extracted with EtOAc (3×10 ml). The combined organic layers were washed several times with water and finally twice with brine. Drying (Na2SO4), filtering and evaporation of the solvent gave the crude product, which was recrystallised from EtOH to afford 24 mg of the title compound as a white solid.

WORKUP

后处理

  1. extractionwas then extracted with EtOAc (3×10 ml)
  2. washThe combined organic layers were washed several times with water
  3. dry with materialDrying (Na2SO4)
  4. filtrationfiltering
  5. customevaporation of the solvent
  6. customgave the crude product, which
  7. customwas recrystallised from EtOH