HRID234708

反应详情

EQUATION

反应方程式

HRID 234708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.16 g (0.39 mMol) of the sulfone of Step 5, 0.2 g of potassium carbonate and 4.0 g of iodomethane, and 5 mL of DMF was stirred for 3 hours, poured into water and extracted with ether. The ether extract was washed with brine, dried over MgSO4 and filtered through silica gel. The filtrate was concentrated in vacuo and the residue was crystallized from hexane to give 5-(4-fluorophenyl)-2-methoxy-4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyridine as a white solid (0.17 g): mp 166.5°-168 ° C.

WORKUP

后处理

  1. extractionextracted with ether
  2. extractionThe ether extract
  3. washwas washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered through silica gel
  6. concentrationThe filtrate was concentrated in vacuo
  7. customthe residue was crystallized from hexane