HRID1617320

反应详情

EQUATION

反应方程式

HRID 1617320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

11.1 g (91.0 mmol) 2-Methyl-2-propanesulfinamide are added to 16.5 g (76.0 mmol) 4-bromo-3-fluoro-benzaldehyde and 34.6 g (152 mmol) titanium(IV) ethoxide in 100 mL THF. Stirring is continued for 1.5 h at 50° C. After that time, the mixture is poured into brine. The mixture is filtered over celite and the filtrate is transferred to a separation funnel. The organic layer is separated, dried over magnesium sulphate and the solvent is removed by evaporation. The residue is purified by column chromatography (silica gel; gradient hexane/EtOAc 1:0→3:2) to yield the desired product.

WORKUP

后处理

  1. filtrationThe mixture is filtered over celite
  2. customthe filtrate is transferred to a separation funnel
  3. customThe organic layer is separated
  4. dry with materialdried over magnesium sulphate
  5. customthe solvent is removed by evaporation
  6. customThe residue is purified by column chromatography (silica gel; gradient hexane/EtOAc 1:0→3:2)