HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | isobutyl P-(3-cyanoprop-2-yl)-P-methyl-phosphinate | HCID 23374761 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate | HCID 23374771 | — |
Reaction Steps
A solution of 29.8 g of isobutyl P-(3-cyanoprop-2-yl)-P-methyl-phosphinate in 200 ml of ethanol is added to 310.0 g of an 8% solution of ammonia in ethanol. To this are added 20 ml of Raney nickel slurry, and the resulting mixture is hydrogenated at 1 bar until hydrogen uptake ceases. The mixture is then filtered and the filtrate is concentrated under reduced pressure. The crude product is distilled under reduced pressure to give isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate, b.p. 100°/0.1 mbar, 31P-NMR spectrum: δ=+58.9 and +58.4 ppm (CDCl3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05567840 |
| Source dataset | uspto-grants-1996_10 |
| ORD ID | ord-ff0d557d4fb147cfad3a2b52fcc4d40c |
| Source note | uspto-grants-1996_10 |