反应 #1100

反应方程式

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

溶剂

methanol

反应条件

后处理

1. 1
   其他until absorption of hydrogen
2. 2
   过滤After filtering
3. 3
   浓缩the filtrate is concentrated
4. 4
   workup.DISSOLUTIONthe product is dissolved in diisopropyl ether
5. 5
   其他Crystallization
6. 6
   workup.ADDITIONon addition of hexane

实验过程

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.

来源