HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Butanol → 3-(Hydroxymethylphosphinyl)propionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Methylphosphonous acid | HCID 77879 | — |
| Product | 3-(Hydroxymethylphosphinyl)propionic acid | HCID 84788 | — |
Reaction Steps
Hydrolysis of Dibutyl Carboxyethylmethylphosphinate 528 g (2 mol) of the dibutyl carboxyethylmethylphosphinate obtained according to Example 4 are charged to a 1 l five-neck flask fitted with thermometer, reflux condenser, high-speed stirrer and dropping funnel. At 160° C., 500 ml of water are metered in over 4 h and a butanol-water mixture is distilled off. 281 g of butanol are obtained, which corresponds to 95% of theory. The distillatively removed butanol is re-used to esterify the methylphosphonous acid. 300 g of carboxyethylmethylphosphinic acid are obtained as a white solid having a melting point of about 95° C. and a 31P NMR purity of >97%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06855757B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-8422a13963d249619fce4f39924e8fa1 |
| Source note | uspto-grants-2005_02 |