Ethanol → Ethyl diphenylphosphinite

Participants

Reaction Steps

The following feed streams were mixed continuously in a reaction mixing pump: 1) mixture of 159.2 g of 1-methylimidazole and 85.4 g of ethanol and 2) 372.8 g of chlorodiphenylphosphine (99.1% strength). Stream 1) was added at 1257 g/h and stream 2) was added at 1928 g/h. The volume of the mixing chamber was 3.3 ml. The top of the reaction mixing pump was thermostated to 120° C. The system was brought to equilibrium over a period of 5 minutes. The output was subsequently collected for 11 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. 372.8 g of chlorodiphenylphosphine were added. The output consisted of two liquid phases. During the 11 minutes, 392.2 g of upper phase and 218.3 g of lower phase were collected. The upper phase comprised 96.5% of EODPP, so that the yield determined by gas chromatography was 98.2%. The residence time of the reactants in the mixing chamber was 4 s, so that the space-time yield was 0.69×106 kgm−3h−1.

Provenance & Evidence