HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → HCID 21866673, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 21866788 | HCID 21866788 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 21866673 | HCID 21866673 | 74.5% |
Reaction Steps
Phosphorus tribromide (6.77 g) was added to 94 ml of a solution of 4.90 g of 2-methyl-2-{6-[5-methyl-2-(p-tolyl)oxazol-4-yl]hexyloxy}propionohydroxamic acid in benzene, and heated to reflux for 4 hours. The reaction solution was cooled, poured into ice-cold water. After addition of saturated aqueous sodium hydrogencarbonate solution, the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine sequentially, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (Wakogel® C-200, n-hexane:ethyl acetate=9:1) to provide 3.32 g of the objective compound as a colorless crystals. M.p. 36° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06998412B2 |
| Source dataset | uspto-grants-2006_02 |
| ORD ID | ord-3705ca3b2d574420968daf2713f5ba34 |
| Source note | uspto-grants-2006_02 |