反应详情

To a solution of the relevant 2-[1-(4-hydroxybutyl)-cyclohex-2-enyl]-N,N-dimethyl-acetamide isomer (6) or (6′) (13.7 g, 57.1 mmol) in DMF (200 mL) was added pyridinium dichromate (65.3 g, 241.0 mmol) and the mixture stirred at room temperature for 24 hours. The reaction mixture was poured into H2O (200 mL) and extracted with EtOAc (5×). The combined organic layers were washed with a saturated NaCl solution and dried over anhydrous MgSO4. The solvent was removed in vacuo, the residual DMF was removed by vacuum distillation (Kugelrohr-type) to afford 13.3 g of the desired product which was used without further purification.

1. extractionextracted with EtOAc (5×)
2. washThe combined organic layers were washed with a saturated NaCl solution
3. dry with materialdried over anhydrous MgSO4
4. customThe solvent was removed in vacuo
5. customthe residual DMF was removed by vacuum distillation (Kugelrohr-type)