反应详情

A solution of ethyl 1-benzyl-4-(N,N'-di-tert-butyloxycarbonylhydrazino)piperidin-4-yl-carboxylate (D26, 14.2 g, 0.030 mol) in methanol (50 ml) was treated with 10% HCl/methanol (100 ml) and heated under reflux for 2 h. The solution was concentrated in vacuo and the residue treated with dry toluene (80 ml) and again concentrated in vacuo to remove any traces of moisture. The residue was trituated with ether and the material filtered off and immediately placed in a vacuum dessicator to give the title compound (D27) (9.48 g, 90%) as a very hygroscopic orange solid.

1. temperatureheated
2. temperatureunder reflux for 2 h
3. concentrationThe solution was concentrated in vacuo
4. additionthe residue treated with dry toluene (80 ml)
5. concentrationagain concentrated in vacuo
6. customto remove any traces of moisture
7. filtrationthe material filtered off