反应详情

A solution of 2 g of 3-oxo-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester, 1.2 ml of cyano-acetic acid methyl ester, 130 μl of piperidine and 38 mg of β-alanine in 4 ml of DMF is stirred at 70° C. for 48 hours, the mixture obtained is diluted with EtAc, washed with H2O and brine, the organic layer obtained is dried, solvent is removed in vacuo and the residue obtained is subjected to chromatography on silica gel. 3-(cyano-methoxycarbonyl-methylene)-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester is obtained in the form of an oil. 13C-NMR: 174.13, 162.27, 153.68, 115.37, 107.45, 80.70, 53.92, 53.08, 28.81.

1. customthe mixture obtained
2. additionis diluted with EtAc
3. washwashed with H2O and brine
4. customthe organic layer obtained
5. customis dried
6. customsolvent is removed in vacuo
7. customthe residue obtained