HRID580402

反应详情

EQUATION

反应方程式

HRID 580402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

α-(2-Propenyl)-[2-(2-nitro-5-trifluoromethylphenyl)-1-(4-methoxyphenyl)ethyl]propanedioic acid, dimethyl ester (50.49 g; 0.102 mole) was dissolved in methanol (350 ml) under argon at room temperature. Powdered stannous chloride dihydrate (119.67 g; 0.53 mole; 5.2 eq.) was added followed by concentrated hydrochloric acid (155 ml with stirring. 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 (rinsed three times with ethyl acetate), rotary evaporated, and suction-filtered. The collected white solid was rinsed with 10% methanol:water and dried giving 51.97 g of the title compound.

WORKUP

后处理

  1. additionwas added portionwise)
  2. filtrationThe suspension was filtered through a Celite pad (rinsed three times with ethyl acetate), rotary evaporated
  3. filtrationsuction-filtered
  4. washThe collected white solid was rinsed with 10% methanol
  5. dry with materialwater and dried