HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethyl phosphite → HCID 10220583, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethyl phosphite | HCID 8472 | — |
| Reactant | 2-Bromomethylnaphthalene | HCID 70320 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 10220583 | HCID 10220583 | 92.6% |
Reaction Steps
A solution of 2-bromomethylnaphthalene (4.42 g, 0.020M) and trimethylphosphite (5 mL, 5.26 g, 0.042M) in dry toluene (100 mL) is heated at reflux temperature for 120 hours The reaction is incomplete, so the volume of the solution is reduced to 25 mL, additional trimethylphosphite (5 mL) is added, and the solution heated to reflux for another 24 hours. Solvent is removed under reduced pressure and the solid white residue is chromatographed over silica gel (40-63 μm, 195 g, ethyl acetate). Elution of the column with ethyl acetate gave title compound (4.63 g) as a white solid which after crystallization from ether-hexane had mp 80°-81° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05593980 |
| Source dataset | uspto-grants-1997_01 |
| ORD ID | ord-ec468e00dd6a4f1290c3afc2c9a892f4 |
| Source note | uspto-grants-1997_01 |