Реакция #1100

Уравнение реакции

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

Растворители

methanol

Условия реакции

Обработка

1. 1
   Другоеuntil absorption of hydrogen
2. 2
   ФильтрацияAfter filtering
3. 3
   Концентрированиеthe filtrate is concentrated
4. 4
   workup.DISSOLUTIONthe product is dissolved in diisopropyl ether
5. 5
   ДругоеCrystallization
6. 6
   workup.ADDITIONon addition of hexane

Методика

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.

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