HRID1704801
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe solution is evaporated to 50 ml
- additiondiluted with ether
- extractionThe resulting solution is extracted three times with 5% sodium carbonate
- extractionThe precipitated product is extracted with ether/methylene chloride (1:3)
- customThe organic extracts are dried
- customevaporated
- customThe residue is recrystallized from ethanol, there