Hydrochloric Acid → Diethyl (2-oxoethyl)phosphonate

Temperature

50 °C

A 2-litre, four-necked flask equipped with a mechanical stirrer, an addition funnel and a nitrogen inlet was charged with diethyl 2,2-diethoxyethylphosphonate (150 g) and water (300 mL), and a slight stream of nitrogen was continuously passed through the system. The resulting mixture was heated to 50° C. and hydrochloric acid (5.6 mL) was added. The mixture was then left under stirring for 4 hours after which water was added and the mixture concentrated under reduced pressure. Sodium chloride was added to the resulting mixture which was then extracted with 4 portions of ethyl acetate. The combined organic phases were distilled under reduced pressure.

1. customA 2-litre, four-necked flask equipped with a mechanical stirrer, an addition funnel and a nitrogen inlet
2. waitThe mixture was then left
3. additionwas added
4. concentrationthe mixture concentrated under reduced pressure
5. additionSodium chloride was added to the resulting mixture which
6. extractionwas then extracted with 4 portions of ethyl acetate
7. distillationThe combined organic phases were distilled under reduced pressure

ORD record

ord-86c160e075344d7488e42d81e3f643e5

Source dataset

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09290439B2