HRID2057104

反应详情

EQUATION

反应方程式

HRID 2057104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 3-methyl-4-[2-[N-isobutyl-N-(5-methyl-2-furylsulfonyl)amino]4,5-dimethylphenoxymethyl]benzoic acid methyl ester prepared in example 1 (850 mg) in dioxane (10 ml), 2N aqueous sodium hydroxide (2.5 ml) and methanol (4 ml) were added, and the mixture was stirred for 30 hours at room temperature. To the mixture, 2N hydrochloric acid was added, then ethyl acetate-water (30 ml-15 ml) was also added. The organic layer was washed, dried and concentrated under reduced pressure. The residue was dissolved in hot ethanol (40 ml) and added by hot water (40 ml), then allowed to cool. Precipitation was filtrated, and dried to give the title compound (755 mg) having the following physical data.

WORKUP

后处理

  1. washThe organic layer was washed
  2. customdried
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in hot ethanol (40 ml)
  5. additionadded by hot water (40 ml)
  6. temperatureto cool
  7. customPrecipitation
  8. filtrationwas filtrated
  9. customdried