HRID1704801

反应详情

EQUATION

反应方程式

HRID 1704801 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

50 g of 3-veratroylpropionic acid in 400 ml of chloroform and 22.7 g of 1,3-propanedithiol are treated with hydrogen chloride up to saturation while stirring. After 3 hours at room temperature, the solution is evaporated to 50 ml and diluted with ether. The resulting solution is extracted three times with 5% sodium carbonate. The basic phases are combined and made acidic with concentrated hydrochloric acid. The precipitated product is extracted with ether/methylene chloride (1:3). The organic extracts are dried and evaporated. The residue is recrystallized from ethanol, there being obtained 2-(3,4-dimethoxyphenyl)-m-dithiane-2-propionic acid of melting point 134°-135° C.

WORKUP

后处理

  1. customthe solution is evaporated to 50 ml
  2. additiondiluted with ether
  3. extractionThe resulting solution is extracted three times with 5% sodium carbonate
  4. extractionThe precipitated product is extracted with ether/methylene chloride (1:3)
  5. customThe organic extracts are dried
  6. customevaporated
  7. customThe residue is recrystallized from ethanol, there