反应 #1076772

反应方程式

2,2-Dimethoxypropane

3,3-Bis(hydroxymethyl)-2-butanone

→

desired product

5-Acetyl-2,2,5-trimethyl-1,3-dioxane

溶剂

dichloromethane

反应条件

后处理

1. 1
   workup.ADDITION40.0 g) was added to the solution

实验过程

2,2-Dimethoxypropane (418.0 g, 4.0 mol) and The 3,3-Bis(hydroxymethyl)-2-butanone (264.32 g, 2.0 mol) were mixed together in 1 liter of dichloromethane. Amberlyst-15 ion exchange resin (strongly acidic; 40.0 g) was added to the solution and the resultant suspension stirred vigorously at room temperature. After 1 hr TLC indicated no starting material and complete conversion to the desired product. The spent resin was separated from the solution by filtration through a thick pad of anhydrous potassium carbonate. Subsequently, the residual dimethoxypropane and dichloromethane were removed in vactio to give a pale straw-colored liquid. The liquid solidified upon standing as large clear, colorless crystals, m.p. 48-50° C.; 300 g, 87.1% of theoretical yield; H-NMR spectra were consistent. Elemental Analysis calculated for C9H16O3: C, 62.77; H, 9.36. Found: C, 62.00; H. 9.01.

来源