HRID1280743

反应详情

EQUATION

反应方程式

HRID 1280743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Bromo-3H-benzooxazol-2-one (0.165 g, 0.77 mmol) was added portionwise into a 0° C. suspension of NaH (44.8 mg, 1mmol, 55%) in dry DMF (4 ml). After 1 hour stirring at room temperature, a solution of triphenylmethylchloride (0.24 g, 0.85 mmol) in DMF (0.5 ml) was added. The reaction mixture was stirred 1 hour at room temperature then quenched with H2O (15 ml). The aqueous phase was extracted with ethyl acetate, the combined organic phases were washed with H2O and brine, dried over Na2SO4 and concentrated to provide 6-bromo -3-trityl-3H-benzooxazol-2-one (0.27 g, 77 %) as a beige solid, MS: m/e=457.1 (M+H+).

WORKUP

后处理

  1. stirringThe reaction mixture was stirred 1 hour at room temperature
  2. customthen quenched with H2O (15 ml)
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. washthe combined organic phases were washed with H2O and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated