Ethanol → Ethyl diphenylphosphinite

Participants

Reaction Steps

The following feed streams were mixed continuously in a reaction mixing pump: 1) mixture of 156.7 g of 1-methylimidazole and 84.1 g of ethanol and 2) 370.0 g of chlorodiphenylphosphine (99.1% strength). Stream 1) was added at 167.5 g/h and stream 2) was added at 257.4 g/h. The volume of the mixing chamber was 3.3 ml. The top of the reaction mixing pump was thermostated to 80° C. The system was brought to equilibrium over a period of 60 minutes. The output was subsequently collected for 87 minutes in order to carry out a mass balance. During the mass balance run, the amount of starting materials was determined by weighing the reservoirs. 370.0 g of chlorodiphenylphosphine were added. The output consisted of two liquid phases. During the 87 minutes, 389.3 g of upper phase and 219.2 g of lower phase were collected. The upper phase comprised 96.8% of EODPP, so that the yield determined by gas chromatography was 98.5%. The residence time of the reactants in the mixing chamber was 30 s.

Provenance & Evidence