HRID580391

反应详情

EQUATION

反应方程式

HRID 580391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

α-Methyl-[2-(2-nitro-5-trifluoromethylphenyl)-1-(4-methoxyphenyl)ethyl]propanedioic acid, dimethyl ester (6.80 g; 14.9 mmole) was dissolved in methanol (200 ml) under argon at room temperature. Powdered stannous chloride dihydrate (17.48 g; 77.5 mmole) was added, followed by concentrated hydrochloric acid (19 ml) with stirring. After 1.5 hours, Celite, ethyl acetate and saturated potassium carbonate solution were added with stirring (the potassium carbonate was added portionwise). The suspension was filtered through a Celite pad. The pad was then rinsed with ethyl acetate (three times). The filtrate was concentrated and the resulting white solid was triturated with 10% methanol:water and dried giving 6.02 g of the title compound.

WORKUP

后处理

  1. additionwas added portionwise)
  2. filtrationThe suspension was filtered through a Celite pad
  3. washThe pad was then rinsed with ethyl acetate (three times)
  4. concentrationThe filtrate was concentrated
  5. customthe resulting white solid was triturated with 10% methanol
  6. dry with materialwater and dried