HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178443526, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl methylphosphonite | HCID 85063 | — |
| Reactant | 1,4,5-Triphenyl-2-(7-bromoheptyloxy)imidazole | HCID 22916412 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178443526 | HCID 178443526 | 57.3% |
Reaction Steps
A solution of 1,4,5-triphenyl-2-(7-bromoheptyloxy)-imidazole (1.75 g) and diethyl methylphosphonite (2.45 g) in toluene (10 ml) was heated at reflux temperature for 48 hours. Methanol and water were added and the mixture evaporated to an oil. This was chromatographed on silica gel (ethyl acetate/ethanol). The resulting oil slowly crystallised and was triturated with ether/petroleum ether, filtered then recrystallised from ethanol/ether to give ethyl 7-(1,4,5-triphenyl-imidazol-2-yloxy)heptane-methylphosphinate (1.06 g, 57%) as a white solid, m.p. 101°-2° C. Found: C, 72.05; H, 7.26; N, 5.52%; C31H37N2O3P; Requires: C, 72.07; H, 7.22; N, 5.42%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05648373 |
| Source dataset | uspto-grants-1997_07 |
| ORD ID | ord-b4e6be7428ea45bfb31e2b127adfab45 |
| Source note | uspto-grants-1997_07 |