HRID470261

反应详情

EQUATION

反应方程式

HRID 470261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of benzyl(4aR,7aR)-2-benzamido-7a-(2-thienyl)-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazine-6-carboxylate (14 g, 29.3 mmol) in acetonitrile (210 mL) is treated with iodotrimethylsilane (7.53 mL, 52.7 mmol) at room temperature. The solution is stirred for 1 hour and the solvent is evaporated. The residue is quenched with 1 M hydrochloric acid and ethyl acetate and the resulting mixture is filtered through diatomaceous earth. The aqueous layer is separated, neutralized with 50% w/w aqueous solution of sodium hydroxide and extracted with ethyl acetate. The organic extracts are dried over sodium sulfate and concentrated to give the title compound (7.9 g, 78%). ES/MS (m/e): 344 (M+H).

WORKUP

后处理

  1. customthe solvent is evaporated
  2. customThe residue is quenched with 1 M hydrochloric acid and ethyl acetate
  3. filtrationthe resulting mixture is filtered through diatomaceous earth
  4. customThe aqueous layer is separated
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic extracts are dried over sodium sulfate
  7. concentrationconcentrated