Reaction #3597528
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06355646B1
Conditions: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: Potassium t-butoxide (Aldrich, 95%, 39.0 g) was added to a solution of tetraethylene glycol (Aldrich, 412.7 g) and methyl hexaethylene glycol chloride from above (95.8 g) at 18° C. over a 25 min period (ice/acetone bath). The reaction mixture was then stirred at 120° C. overnight. The pH was adjusted to 7 by the addition of hydrochloric acid (12 N, 11.7 ml), and volatiles were removed (64 Pa (0.48 Torr), up to 185° C.). The residual dark oil was diluted with toluene (250 ml), and treated with calcium chloride (38.1 g). After stirring for 18 h, the mixture was filtered through Celite™ and concentrated to a dark oil (102 g), which was fractionally distilled to provide decaethylene glycol monomethyl ether as an amber oil (64.4 g, 45%). were removed (64 Pa (0.48 Torr) up to 185° C. The residual dark oil was diluted with toluene (250 ml) treated with calcium chloride (38.1 g) After stirring for 18 h the mixture was filtered through Celite™ concentrated to a dark oil (102 g), which was fractionally distilled
Source ID: ord-ddecdbd18791432fbc980e552acef82f