Water → HCID 86757620, compound

Participants

Reaction Conditions

Reaction Steps

In 18.74 kg of dimethyl formamide (DMF) was added 11.48 kg of phosphorus oxychloride at 10° C., and stirred at the same temperature for 1 hour. To the sticky solution thus obtained was added 25 l of a solution of 6.0 kg (31.9 mol) of 1,1-diethoxyheptane in dichloromethane at 10° C., stirred at the same temperature for 2 hours, and then heated up to 70° C. in 30 min. The reaction solution was cooled down, gradually added to an aqueous solution of 33.2 kg of potassium carbonate and 100 l of water so that the temperature did not exceed 30° C., and then stirred at room temperature for 5 hours. The product was extracted with chloroform. The extract was washed with saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was distilled off under a reduced pressure, and the residue was purified by distillation to obtain 2.6 kg (15.3mol) of 2-ethoxymethylidenylheptanal. Yield of this product was 48%.

Provenance & Evidence