HRID734657

反应详情

EQUATION

反应方程式

HRID 734657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureheated
  2. temperatureto reflux for 4 hours
  3. customto the cooled reaction mixture
  4. filtrationThe solid was collected by filtration
  5. customtriturated with diethyl ether