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
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
435 g of benzaldehyde and 550 g 2,2-bis(hydroxymethyl)propanoic acid were allowed to react in the presence of a small amount of p-toluenesulphonic acid. The reaction was under stirring carried out at room temperature followed by heating to 40° C. under a low pressure (15 mm Hg). Yielded product was then dissolved in a mixture of 8000 ml aqueous sodium hydrogencarbonate (0.54M) and 2500 ml of diethyl ether. The aqueous phase was now washed with diethyl ether and acidified with 800 g of tartaric acid. The precipitate was collected and washed with water. Obtained product was finally recrystallized from ethanol/ethyl acetate to yield 745 g of 5-methyl-2-phenyl-1,3-dioxane-5-carboxylic acid.
WORKUP
后处理
- customcarried out at room temperature
- washThe aqueous phase was now washed with diethyl ether
- customThe precipitate was collected
- washwashed with water
- customObtained product was finally recrystallized from ethanol/ethyl acetate