HRID48969

反应详情

EQUATION

反应方程式

HRID 48969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 3-[3-[3-(bromomethyl)-2-thienyl]-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)uracil(1.00 g, 1.99 mmol), methylene chloride and methanol is added silver trifluorormethanesulfonate. The resultant white suspension is stirred overnight at room temperature and filtered through a pad of diatomaceous earth with methylene chloride wash. The filtrate is washed with saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to a pale yellow solid, which is recrystallized from diethyl ether to afford the title compound (0.790 g, 87.7%, mp 131-133° C.) which is identified by NMR spectral analysis.

WORKUP

后处理

  1. filtrationfiltered through a pad of diatomaceous earth with methylene chloride
  2. washwash
  3. washThe filtrate is washed with saturated sodium bicarbonate and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo to a pale yellow solid, which
  6. customis recrystallized from diethyl ether