HRID400229

反应详情

EQUATION

反应方程式

HRID 400229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred mixture of ortho-hydroxycinnamic acid (1.00 g, 6.09 mmol) in 10 mL of ether and 10 mL of methanol was added etheral diazomethane until the mixture became yellowish. The mixture was stirred at room temperature for 15 minutes, and the excess diazomethane was destroyed with the addition of acetic acid. The mixture was concentrated in vacuo and diluted with 100 mL of ethyl acetate. This ethyl acetate solution was washed with saturated sodium bicarbonate solution (3×60 mL) and brine (1×60 mL). The organic layer was dried (magnesium sulfate), filtered and concentrated in vacuo to give 1.02 g (94%) of methyl ortho-hydroxycinnamate B.

WORKUP

后处理

  1. customthe excess diazomethane was destroyed with the addition of acetic acid
  2. concentrationThe mixture was concentrated in vacuo
  3. additiondiluted with 100 mL of ethyl acetate
  4. washThis ethyl acetate solution was washed with saturated sodium bicarbonate solution (3×60 mL) and brine (1×60 mL)
  5. dry with materialThe organic layer was dried (magnesium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo