Potassium Iodide → Carbomethoxymethyl 2,2-bis-(hydroxymethyl)-propionate

Temperature

100 °C

A 5-liter reaction vessel which has been equipped with a stirrer, an internal thermometer, a reflux condenser and a 1-liter dropping funnel is charged with 550 g of 2,2-bis-(hydroxymethyl)-propionic acid and 2,460 g of cyclohexanone, and the mixture is heated to 100° C. When the bulk of the dihydroxycarboxylic acid has gone into solution, the temperature is lowered to 60° C., and 414 g of triethylamine are added dropwise. The temperature is held at 60° C. by cooling. The resulting triethylammonium 2,2-bis-(hydroxymethyl)-propionate stays in solution. 7 g of potassium iodide are then added, followed, in dropwise fashion, by 565 g of methyl chloroacetate in the course of 30 minutes. The batch is held at this temperature for a further 4 hours, is then allowed to cool down to room temperature and is filtered to remove the triethylammonium chloride formed. The filtrate is concentrated in a rotary evaporator and is then adjusted with xylene to a solids content of 90%.

1. customA 5-liter reaction vessel which
2. customhas been equipped with a stirrer
3. customis lowered to 60° C.
4. customis held at 60° C.
5. temperatureby cooling
6. temperatureto cool down to room temperature
7. filtrationis filtered
8. customto remove the triethylammonium chloride
9. customformed
10. concentrationThe filtrate is concentrated in a rotary evaporator

ORD record

ord-b05d94b324fe497bb77ef6a7d76ce2a2

Source dataset

uspto-grants-1984_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04477642