HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → HCID 22981310, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | tert-butyl N-[4-(hydroxymethyl)-2-methylphenyl]carbamate | HCID 22981315 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22981310 | HCID 22981310 | 36.4% |
Reaction Steps
The compound (1.035 g) obtained in Example 518 was dissolved in methylene chloride (20 ml) and to the solution, triphenylphosphine (1.38 g) and carbon tetrabromide (1.74 g) were successively added under ice cooling. The reaction mixture was stirred for 30 min under ice cooling, then stirred at room temperature for 30 min and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=5:1) to give 476.6 mg of the titled compound (yield, 36%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06534546B1 |
| Source dataset | uspto-grants-2003_03 |
| ORD ID | ord-4a27f0bff4a0406d827c1f1f587b975d |
| Source note | uspto-grants-2003_03 |