Hydrochloric Acid → 3,3-Diethoxypropanoic acid

Temperature

100 °C

To a 250 mL round-bottomed flask with magnetic stirring that contained ethyl 3,3-diethoxypropanoate (20.0 g, 102.0 mmol, colourless oil, 97%), a previously prepared solution of NaOH (5.23 g, 131.0 mmol) in H2O (30 mL) was added. The resulting mixture was stirred to reflux (100° C.) during 1 h. After allowing it to temper, the mixture was acidified using HCl 37% and it was extracted with AcOEt, 8×20 mL. The resulting organic phase was washed with 1×20 mL NaCl sat., dried with Na2SO4, filtered and concentrated to dryness. The obtained oil was confirmed to correspond to the title compound (15.9 g, 98.0 mmol, 96%).

1. stirringThe resulting mixture was stirred
2. extractionwas extracted with AcOEt, 8×20 mL
3. washThe resulting organic phase was washed with 1×20 mL NaCl sat.
4. dry with materialdried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated to dryness

ORD record

ord-a441bb7ef5fd48638d3a2ac6a1e075ff

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09035070B2