Ethanol → Ethyl diphenylphosphinite

Participants

Reaction Conditions

Reaction Steps

The following starting materials were fed continuously at 80° C. into a reactor which was equipped with a three-stage inclined-blade stirrer and had been made inert with nitrogen: 1) mixture of 110.7 g of ethanol and 205.8 g of 1-methylimidazole and 2) chlorodiphenylphosphine (99.4% strength). Stream 1) was added at 330 ml/h and stream 2) was added at 380 ml/h. Both streams were introduced below the surface of the liquid. The reactor was equipped with an overflow from which reaction mixture could flow out continuously. The reactor volume up to the overflow was 710 ml. The reaction temperature was maintained at 80° C. To bring the system to equilibrium, the output obtained over the first 4 hours was discarded. The output was subsequently collected over a period of 1 hour and a mass balance was carried out. The output consisted of two liquid phases. Over a period of one hour, 497.2 g of upper phase and 280.8 g of lower phase were collected. The upper phase comprised 96.8% of EODPP. The upper phase was subsequently distilled under reduced pressure via a column filled with Raschig rings, giving 438.2 g of 99.74% strength EODPP. Together with the EODPP in the first fraction, the total yield was 96.7%.

Provenance & Evidence