反应详情

A solution of the crude 4-benzyl-2-methyl-morpholine-3-carboxylic acid ethyl ester (Comp. No. 26) obtained in the preceding experiment in methanol (10 ml) was treated with a catalytic amount of palladium on charcoal (10% w/w; 25 mg). The flask was flushed with hydrogen and the hydrogen atmosphere was maintained whilst stirring at room temperature. After 5 h, the catalyst was removed by filtration, the solution was treated with a new amount of palladium on charcoal (10% w/w; 25 mg) and the hydrogen atmosphere was restored. Stirring was continued for a further 96 h. The catalyst was filtered off, washed with methanol and the combined filtrates were concentrated in vacuo to give 0.140 g of 2-methyl-morpholine-3-carboxylic acid ethyl ester, which was used in the next step without further purification. LC/MS (method 7): Rt=0.45 min; m/z=174.15 (M+H+).

1. customThe flask was flushed with hydrogen
2. temperaturethe hydrogen atmosphere was maintained
3. customthe catalyst was removed by filtration
4. additionthe solution was treated with a new amount of palladium on charcoal (10% w/w; 25 mg)
5. stirringStirring
6. waitwas continued for a further 96 h
7. filtrationThe catalyst was filtered off
8. washwashed with methanol
9. concentrationthe combined filtrates were concentrated in vacuo