Pyridine → HCID 15009139, compound

Temperature

0 °C

To a well-stirred solution consisting of 34.40 g. (0.20 mole) of 2-iodoethanol dissolved in 25 ml. of benzene precooled to 0° C. with the aid of an ice/water bath, there is added in a dropwise manner a solution consisting of 19.1 ml. (0.20 mole) of ethyl chloroformate dissolved in 25 ml. of benzene. Upon completion of this step, the reaction mixture is treated with 19.1 ml. (0.20 mole) of pyridine which is also added in a dropwise manner. The resulting suspension is then stirred for a period of one hour at 0° C. (while under a nitrogen atmosphere) and for six hours at room temperature (~20° C.). At the end of this time, the pyridine hydriodide is removed by filtration and the organic filtrate is washed twice with 50 ml. of 3N hydrochloric acid and once with 50 ml. of brine, followed by drying over anhydrous magnesium sulfate. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there is obtained 2-iodoethyl ethyl carbonate as the residual material.

1. additionthere is added in a dropwise manner a solution
2. additionUpon completion of this step, the reaction mixture is treated with 19.1 ml
3. customAt the end of this time, the pyridine hydriodide is removed by filtration
4. washthe organic filtrate is washed twice with 50 ml
5. dry with materialby drying over anhydrous magnesium sulfate
6. customAfter removal of the drying agent
7. filtrationby means of filtration
8. customthe solvent by means of evaporation under reduced pressure

ORD record

ord-78b09d47d30e4d7bb0bd87729773732c

Source dataset

uspto-grants-1992_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05081118