반응 #1100

반응 방정식

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

용매

methanol

반응 조건

후처리

1. 1
   기타until absorption of hydrogen
2. 2
   여과After filtering
3. 3
   농축the filtrate is concentrated
4. 4
   workup.DISSOLUTIONthe product is dissolved in diisopropyl ether
5. 5
   기타Crystallization
6. 6
   workup.ADDITIONon addition of hexane

실험 절차

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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