HRID403372

反应详情

EQUATION

反应方程式

HRID 403372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-methanesulfonyl-5-trifluoromethyl-benzoic acid methyl ester (1.0 g, 3.54 mmol) in dioxane (15 mL) was added water (15 mL) and lithium hydroxide monohydrate (186 mg, 4.43 mmol). The reaction mixture was stirred at room temperature for 2 hours and then poured on 100 ml 1M aqueous hydrochloric acid and 100 mL ethyl acetate. The layers were separated and the aqueous layer was extracted a second time with 100 mL ethyl acetate. The organic layers were washed with 100 mL brine, dried over magnesium sulfate, filtered and concentrated under vacuum. Colorless solid (930 mg, 98%). MS (ESI−): m/z=266.995 ([M−H]−).

WORKUP

后处理

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted a second time with 100 mL ethyl acetate
  3. washThe organic layers were washed with 100 mL brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum