反应详情

A mixture of 16.0 g (0.05 mol) of 1-(9H-fluoren-9-ylmethoxycarbonyl)-4-piperidinone, 7.25 g (0.055 mol) of tert. butyl hydrazinoformate and 250 ml of ethanol was refluxed for 1 hour. The solvent was distilled off in vacuo, the oily residue remaining was triturated with diethylether. The crystalline precipitate thus formed was suction filtered and washed with a little diethylether. After the product had been dried in vacuo 21.7 g (99.7% of theory) of colourless crystals were obtained, m.p. 156-158° C. (decomposition).

1. temperaturewas refluxed for 1 hour
2. distillationThe solvent was distilled off in vacuo
3. customthe oily residue remaining was triturated with diethylether
4. customThe crystalline precipitate thus formed
5. filtrationfiltered
6. washwashed with a little diethylether
7. customAfter the product had been dried in vacuo 21.7 g (99.7% of theory) of colourless crystals
8. customwere obtained