반응 #1824308

반응 방정식

hydrogen

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

→

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

용매

methanol

반응 조건

후처리

1. 1
   workup.DISSOLUTIONare dissolved
2. 2
   기타After the autoclave has been closed
3. 3
   workup.ADDITION1.3 g of active carbon is added under nitrogen to the warm solution
4. 4
   여과the catalyst is filtered off
5. 5
   workup.ADDITION42 g of 70% sulfuric acid are added dropwise to the solution
6. 6
   기타The product precipitated
7. 7
   여과is filtered off under suction
8. 8
   세척washed with methanol
9. 9
   기타dried

실험 절차

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.

출처