1-Butanol → Acetic acid, 2-butoxy-2-hydroxy-, butyl ester

Participants

Reaction Conditions

Reaction Steps

In a suitable reactor flask equipped with stirrer, heating mantle, Dean Stark trap, condenser, nitrogen inlet, vacuum take off and dropping funnel were added 1980 grams (13.0 moles) of 50% glyoxylic acid in water and 1215 grams (16.4 moles) of n-butanol. The contents of the flask were heated to 80-85° C. under nitrogen sparge and vacuum to remove approximately 760 grams of an n-butanol/water azeotrope. Thereafter, an additional 1210 grams of n-butanol were added and strip distillation continued until no water was seen in the azeotrope. An additioral 810 grams of n-butanol were then added and the mixture refluxed for two hours at 80-85° C. under vacuum, followed by vacuum stripping of excess n-butanol. Product weight was 2850 grams.

Provenance & Evidence