反应 #1824308

反应方程式

hydrogen

4-(2,4-dinitrophenoxymethyl)-2,2-dimethyl-1,3-dioxolane

→

4-(2,4-diaminophenoxymethyl)-2,2-dimethyl-1,3-dioxolane

溶剂

methanol

反应条件

后处理

1. 1
   workup.DISSOLUTIONare dissolved
2. 2
   其他After the autoclave has been closed
3. 3
   workup.ADDITION1.3 g of active carbon is added under nitrogen to the warm solution
4. 4
   过滤the catalyst is filtered off
5. 5
   workup.ADDITION42 g of 70% sulfuric acid are added dropwise to the solution
6. 6
   其他The product precipitated
7. 7
   过滤is filtered off under suction
8. 8
   洗涤washed with methanol
9. 9
   其他dried

实验过程

215 ml of methanol are introduced into a 0.7 l autoclave, 85.3 g (0.3 mole) of 4-(2,4-dinitrophenoxymethyl)-2,2-dimethyl-1,3-dioxolane (step a) are dissolved therein and 0.6 g of palladium on active carbon 10% (Degussa) is added. After the autoclave has been closed and blanketed with nitrogen, hydrogenation is carried out under a pressure of 4 bar and at a temperature of 35 to 40° C. until no more hydrogen is taken up. 1.3 g of active carbon is added under nitrogen to the warm solution and the catalyst is filtered off. 42 g of 70% sulfuric acid are added dropwise to the solution while cooling with ice at 5° C. The product precipitated is filtered off under suction, washed with methanol and dried.

来源