反应详情

5-Nitro-2,2-ethylenedioxypentane (103 g) is dissolved in methanol (2.0 l) and initially introduced into a hydrogenation flask. After the thorough flushing of the apparatus with N2, 10% Pd/C (10 g) is added. Hydrogenation is then carried out at RT under normal conditions in a stream of H2 for a total of 11 h with vigorous stirring. After the reaction is complete (TLC dichloromethane/methanol=9:1, staining reagent 1.0% strength ethanolic ninhydrin solution), the flask is flushed with N2 and the mixture is filtered off with suction through kieselguhr. The colorless filtrate is concentrated to dryness at T≦40° C. and p≧30 mbar, the title compound (85 g, quant.) first being obtained as a colorless oil, which solidifies to give a wax. TLC (dichloromethane/methanol=9:1), Rf=0.0 -0.22.

1. additioninitially introduced into a hydrogenation flask
2. customAfter the thorough flushing of the apparatus with N2, 10% Pd/C (10 g)
3. additionis added
4. customis then carried out at RT under normal conditions in a stream of H2 for a total of 11 h with vigorous stirring
5. customthe flask is flushed with N2
6. filtrationthe mixture is filtered off with suction through kieselguhr
7. concentrationThe colorless filtrate is concentrated to dryness at T≦40° C. and p≧30 mbar