Réaction #1100

Équation de réaction

4-[O-benzyl-N-(3,3-dimethyl-1,5-dioxaspiro[5.5]undec-9-yl)hydroxylamino]-3-methoxy-2-methylpyridine

→

4-(3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamino)-3-methoxy-2-methylpyridine

Solvants

methanol

Conditions de réaction

Traitement

1. 1
   Autreuntil absorption of hydrogen
2. 2
   FiltrationAfter filtering
3. 3
   Concentrationthe filtrate is concentrated
4. 4
   workup.DISSOLUTIONthe product is dissolved in diisopropyl ether
5. 5
   AutreCrystallization
6. 6
   workup.ADDITIONon addition of hexane

Mode opératoire

6.5 g of 4-[O-benzyl-N-(3,3-dimethyl-1,5-dioxaspiro[5.5]undec-9-yl)hydroxylamino]-3-methoxy-2-methylpyridine in 70 ml of methanol are hydrogenated using 2 g of Raney nickel at normal pressure until absorption of hydrogen is complete. After filtering, the filtrate is concentrated and the product is dissolved in diisopropyl ether. Crystallization takes place on addition of hexane. 4.3 g=90%; m.p.: 45° C.

Source