1-Butyl-1-methylpiperidinium hexafluorophosphate synthesis

Yield:1257647-66-7 94.6%

Reaction Conditions:

with potassium hexafluorophosphate in dichloromethane;water;Flow reactor;

Steps:

A. Reactions carried out in a packed column in the form of a solid

General procedure: Dichloromethane solutions (anhydrous dichloromethane) of the appropriate starting ionic liquid at a concentration of 0.01M were prepared before the start of each reaction. This solution was dispensed from a half-liter glass bottle. In the case of the filling, which was solid, it was carefully poured through the top inlet into the column until a layer 10 cm high was formed. The solution was pumped at a rate of 25 ml/min for the time over which 100 ml of solution was dosed (volume greater than the volume of the unpacked column). Then, after this time, four samples of the phase were collected in Eppendorf tubes, which left the column through the tap located in its lower part (3 ml each, they were used to perform the IC analysis, Scheme S2). Each of the collected samples Scheme S2. Construction of a system for carrying out the ion exchange reaction in the flow. The reactor was a packed solid column. The system consisted of: (i) a Varian PrepStar SD-1 Pump HPLC, (ii) a packed glass column, and (iii) receivers. [cat] [Y] - starting ionic liquid, AX - compound being the source of the exchanged anion, [cat] [X] - reaction product. was analyzed on IC.

References:

Pawlowska-Zygarowicz, Anna [Tetrahedron Letters,2021,vol. 86,art. no. 153500] Location in patent:supporting information