HRID734657
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
2-Naphthaldehyde (30.0 g, 192 mmol, 1.00 equiv), 2,2-dimethyl-1,3-dioxane-4,6-dione (27.6 g, 192 mmol, 1.00 equiv), methyl acetoacetate (20.7 mL, 192 mmol, 1.00 equiv), and ammonium acetate (15.6 g, 202 mmol, 1.05 equiv) were dissolved in acetic acid (0.20 L) and heated to reflux for 4 hours, then cooled to room temperature. Addition of water (1 L) to the cooled reaction mixture induced formation of a white precipitate. The solid was collected by filtration and triturated with diethyl ether to provide the 20.5 g (36%) of the product as an off-white solid. MS (ES+) m/e 296 [M+H]+.
WORKUP
后处理
- temperatureheated
- temperatureto reflux for 4 hours
- customto the cooled reaction mixture
- filtrationThe solid was collected by filtration
- customtriturated with diethyl ether