HRID1108162

反应详情

EQUATION

反应方程式

HRID 1108162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a well-stirred mixture of 0.6 g of 25% aqueous NaOH, 70 mg of tetrabutylammonium bromide (TBAB) and 10 mL of toluene was added 1.0 g of (+/-)-N-[2-chloro -1-[4'-[(difluoromethyl)thio][1,1'-biphenyl]-4-yl]ethyl]-2,6-difluorobenzamide as a solid. After 45 min, 2 mL of water was added along with 10 mL of diethyl ether. The organic phase was washed with water, dried (MgSO4), filtered, and concentrated to dryness. The residue was triturated with hexanes, filtered, and suction-dried to afford 0.70 g of product, m.p. 75-77° C. The 1H-NMR (CDCl3) spectrum was the same as that the product of Example 6.

WORKUP

后处理

  1. washThe organic phase was washed with water
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated to dryness
  5. customThe residue was triturated with hexanes
  6. filtrationfiltered
  7. customsuction-dried