HRID1406284

反应详情

EQUATION

反应方程式

HRID 1406284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 4-bromo-2-(methylsulfonyl)benzoate (774 mg, 2.64 mmol) in anhydrous THF (10 mL) was added NaH (60% in mineral, 111 mg, 2.77 mmol). The mixture was stirred at room temperature for 5 hr. The reaction was monitored by LCMS for completion. H2O (1 mL) was added to quench the reaction followed by the addition of aqueous hydrochloric acid (1N, 50 mL) and EtOAc (50 mL). The organic layer was separated, and the water layer was extracted with 2×EtOAc. The combined organic layers were washed with brine, dried over sodium sulfate, filtered, and concentrated to give the title compound (689 mg, 100%) as a white solid.

WORKUP

后处理

  1. customto quench the reaction
  2. additionfollowed by the addition of aqueous hydrochloric acid (1N, 50 mL) and EtOAc (50 mL)
  3. customThe organic layer was separated
  4. extractionthe water layer was extracted with 2×EtOAc
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated