Diethyl benzylphosphonate → Benzylphosphonic Acid

Benzylphosphonic acid was prepared as follows. 200.40 g (878 mmoles) of diethyl benzylphosphonate was combined with 350 ml of distilled water and 350 ml of concentrated (~12 molar) hydrochloric acid. The resulting suspension was heated to reflux under nitrogen for 20 hours, whereupon a clear colorless solution was obtained. From this solution, 130 ml of aqueous distillate was removed. The residue was allowed to cool, forming a thick white slurry which was cooled in situ with an ice bath. The slurry was then filtered dry under vacuum, but not washed due to its fairly high solubility in water. The wet solid was then dried in a vacuum at 120° C. overnight. 123.37 g (82% yield) was obtained.

1. concentrationof concentrated (~12 molar) hydrochloric acid
2. temperatureThe resulting suspension was heated
3. temperatureto reflux under nitrogen for 20 hours, whereupon a clear colorless solution
4. customwas obtained
5. customFrom this solution, 130 ml of aqueous distillate was removed
6. temperatureto cool
7. customforming a thick white slurry which
8. temperaturewas cooled in situ with an ice bath
9. filtrationThe slurry was then filtered
10. customdry under vacuum
11. washnot washed due to its fairly high solubility in water
12. customThe wet solid was then dried in a vacuum at 120° C. overnight
13. custom123.37 g (82% yield) was obtained

ORDレコード

ord-b0a253fc7eed4a4d904cc06f8d5f35a1

出典データセット

uspto-grants-1999_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05868959