Sodium Chloride → HCID 11052031, compound

Temperature

0 °C

To a 1-liter, 4-necked round-bottomed flask, equipped with a mechanical stirrer, nitrogen inlet, internal thermometer, addition funnel and cooling bath (-20° to -25° C.), is added 288.4 g (4.0 mol) of 2-methoxypropene and 0.502 g (0.0002 mol) of the pyridinium salt of p-toluene sulfonic acid. To the cooled solution is then slowly added, under a nitrogen flow over a period of 1 hour, 189.0 g (2.0 mol) of 3-chloropropanol. The reaction mixture is then stirred at -20° to -25° C. for 1 hour and then warmed to 0° C. To the reactor is then added a mixture of 25 ml of a saturated aqueous sodium bicarbonate solution and 425 ml of a saturated aqueous sodium chloride solution. The resultant mixture is then transferred to a separatory funnel and the layers are separated. The organic layer is then concentrated in vacuo at 40° C. and the resultant clear light oil is dried at room temperature under high vacuum for 3 hours to yield the desired compound (97.4% yield; and 98.06% purity).

1. customTo a 1-liter, 4-necked round-bottomed flask, equipped with a mechanical stirrer, nitrogen inlet
2. additioninternal thermometer, addition funnel
3. temperaturecooling bath (-20° to -25° C.)
4. additionTo the cooled solution is then slowly added, under a nitrogen flow over a period of 1 hour
5. additionTo the reactor is then added
6. customthe layers are separated
7. concentrationThe organic layer is then concentrated in vacuo at 40° C.
8. customthe resultant clear light oil is dried at room temperature under high vacuum for 3 hours

ORD record

ord-a5626a9fcf6e48debc01001319c70fe3

Source dataset

uspto-grants-1993_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05208352