反应详情

温度

20 °C

135.0 g (417 mmol) 4-(1-diphenylmethylpiperidin-4-yl)-butan-1-ol, 109.5 g (417 mmol) triphenylphosphine and 61.3 g (417 mmol) phthalimide are suspended in THF and 72.6 g (417 mmol) azodicarboxylic acid diethyl ester are added dropwise within 2½ hours under protective atmosphere and light cooling (ca. 15-25° C.). After a further hour, the solvent is removed under vacuum and the residue is crystallized three times from acetic acid ester (1000 ml, 1200 ml and 1100 ml). Colorless crystals with a MP of 150-152 were recovered. Yield 103 g (54.5%).

1. waitAfter a further hour
2. customthe solvent is removed under vacuum
3. customthe residue is crystallized three times from acetic acid ester (1000 ml, 1200 ml and 1100 ml)
4. customColorless crystals with a MP of 150-152 were recovered