HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus pentachloride → HCID 57672582, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 4620448 | HCID 4620448 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57672582 | HCID 57672582 | 71% |
Reaction Steps
6.3 g (30 mmol) of phosphorus pentachloride was added to a mixture of 40 ml of toluene and 4 ml of dioxane containing 4.7 g (21 mmol) of N-cyclopropyl-3-methyl-4-nitrobenzamide and the mixture was heated to reflux for three hours. The reaction mixture was concentrated under reduced pressure, then dissolved in 30 ml of DMF and slowly added dropwise to a DMF solution containing 2.8 g (43 mmol) of sodium azide. The reaction mixture was stirred for five hours, then poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was filtered and washed with ether to obtain 3.7 g of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994339B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-683b3115c8a34b9e8830f03101c9d50c |
| Source note | uspto-grants-2011_08 |