Hydrochloric Acid → 1,1'-Oxybis[2-(2-chloroethoxy)ethane]

A mixture of 430 g of tetraethylene glycol (2.2 moles), 2000 ml of dry benzene, and 386 g of pyridine (4.9 moles) is heated to reflux, and 580 g of thionyl chloride (4.9 moles) is added dropwise with stirring in three hours. During this period the reflux temperature of the mixture drops from 86° to 78°, and a white precipitate is formed. Heating is continued overnight (16 hours) and, after cooling, 50 ml of hydrochloric acid diluted with 200 ml of water is added dropwise in about 15 minutes. Benzene is removed from the upper layer containing the product, and the residue vacuum distilled at 4.5 mm Hg at 165°. The yield is 375 g of light yellow liquid (72%).

1. temperatureis heated
2. temperatureto reflux
3. waitDuring this period the reflux temperature of the mixture drops from 86° to 78°
4. customa white precipitate is formed
5. temperatureHeating
6. waitis continued overnight
7. temperature(16 hours) and, after cooling
8. additionis added dropwise in about 15 minutes
9. customBenzene is removed from the upper layer
10. additioncontaining the product
11. distillationthe residue vacuum distilled at 4.5 mm Hg at 165°

ORD-Eintrag

ord-a20294d38c7f4a97a6d417e365d693e9

Quelldatensatz

uspto-grants-1980_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04196250