HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethyl phosphite → HCID 53693742, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethyl phosphite | HCID 8472 | — |
| Reactant | 2,3-Bis(bromomethyl)naphthalene | HCID 262259 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 53693742 | HCID 53693742 | 97.8% |
Reaction Steps
A flask is charged with 2,3-bis(bromomethyl)naphthalene (Example 22(b), 2.80 g, 8.9 mmol) and toluene (50 mL). The solution is heated at reflux and 25 mL of the toluene is collected in a Dean-Stark trap. The solution is then cooled to room temperature and trimethylphosphite (4.0 mL, 0.034 mol) is added. The reaction is heated to reflux temperature for 24 hours. The excess trimethylphosphite and toluene are removed at reduced pressure, giving a white solid (3.24 g). The solid is recrystallized from ethyl acetate-hexane to give 2.55 g of white crystals, mp 119.5°-120.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05298498 |
| Source dataset | uspto-grants-1994_03 |
| ORD ID | ord-b6ff4fede09d45659eea1b973a38a3ba |
| Source note | uspto-grants-1994_03 |