HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allyl Alcohol → Ethyl-3-hydroxypropylphosphinic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allyl Alcohol | HCID 7858 | — |
| Reactant | Sodium Persulfate | HCID 62655 | — |
| Reactant | Ethylphosphonous acid | HCID 13411864 | — |
| Solvent | Water | HCID 962 | — |
| Product | Ethyl-3-hydroxypropylphosphinic acid | HCID 86656674 | 89% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
564 g (6 mol) of ethylphosphonous acid (produced as in Example 1) are dissolved in 860 g of water and initially charged to a 5 l five-neck flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel. The reaction mixture is heated to 100° C. and 406 g (7 mol) of allyl alcohol and 500 g of a 5% sodium peroxodisulfate solution (1.5 mol % based on allyl alcohol) is added dropwise at atmospheric pressure over 1 h. Then, the water is distilled off in vacuo, and the residue is taken up in tetrahydrofuran and the insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo to leave 812 g (89% of theory) of ethyl(3-hydroxypropyl)phosphinic acid as oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08614267B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-ecff7705adbe4157a25b5afb2e80593f |
| Source note | uspto-grants-2013_12 |