HRID541192

反应详情

EQUATION

反应方程式

HRID 541192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 5-cyano-2,4-dimethylbenzoate (compound 2.3, 6 g, 28.54 mmol, 1.00 equiv, 90%) and NH2OH (10 mL, 5.00 equiv, 50% in water) in EtOH (20 mL) was stirred at 100° C. in an oil bath. After 2 h, the mixture was cooled to room temperature and concentrated under reduced pressure. The residue was diluted with 100 mL of ethyl acetate, washed with 2×20 mL of brine, dried (Na2SO4), and concentrated under reduced pressure to yield 4.66 g (66%) of the title compound as a white solid.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additionThe residue was diluted with 100 mL of ethyl acetate
  3. washwashed with 2×20 mL of brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated under reduced pressure