1-Dodecanol → 1-Chlorododecane

Participants

Reaction Conditions

Reaction Steps

Into a reactor system in accordance with FIG. 1 there were pumped jointly per hour 1.65 kg lauryl alcohol (purity: 97%) and 0.41 kg phosphorus trichloride. The cooling was performed in reaction zone 1 in such a way that the outlet temperature was about 110° C. The residence time in reaction zone 1 was 5 minutes. Following preheating to 150° C for 2.5 minutes, the reaction mixture reached reaction zone 2 in which the reaction temperature was maintained with superheated steam at 165° C. The residence time in reaction zone 2 was 26 minutes. By means of a pressure maintenance valve, the entire reactor system was under a pressure of 30 atm. The product obtained in this manner separated out immediately into two phases. One obtained per hour 1.8 kg of the organic phase corresponding to a yield of 97.5% of lauryl chloride with respect to lauryl alcohol. The purity amounted to 95 weight-percent of lauryl chloride. The product contained 0.14 weight-percent of dilauryl ether. Space-time yield: 1.4 kg/hour, liter.

Provenance & Evidence