HRID541738

反应详情

EQUATION

反应方程式

HRID 541738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-nitro-5-[(trimethylsilyl)ethynyl]benzoate (7.9 g, 28 mmol) was dissolved in THF (90 mL) and methanol (90 mL) and then potassium carbonate (2.0 g, 14 mmol) was added. The resulting solution was stirred at room temperature for 1 hour. The reaction was quenched with 1 N HCl, and the solvent was removed in vacuo. The aqueous residue was extracted with ethyl acetate twice. The combined organic solutions were washed with brine, dried over Na2SO4, filtered and concentrated to give a solid. The solid was washed with ether to give the desired product (4 g, 68%). LCMS for C10H8NO4 (M+H)+: m/z=206.0.

WORKUP

后处理

  1. customThe reaction was quenched with 1 N HCl
  2. customthe solvent was removed in vacuo
  3. extractionThe aqueous residue was extracted with ethyl acetate twice
  4. washThe combined organic solutions were washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give a solid
  9. washThe solid was washed with ether