HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 54324264, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Reactant | Water ethylacetate | HCID 22728543 | — |
| Reactant | HCID 70028635 | HCID 70028635 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 54324264 | HCID 54324264 | — |
Reaction Steps
To a solution of 5-(4-tert-butoxycarbonyl-piperazin-1-yl)-2-chloro-benzoic acid lithium salt (2.1 g) in N,N-dimethylformamide (50 ml) was added diphenyl phosphorylazide (1.4 ml) and reaction mixture stirred at ambient temperature for 1 hour. Water (30 ml) was added and the reaction mixture heated to 60° C. for 2 hours. After cooling to room temperature, the reaction was poured into ethyl acetate/water, the organic layer separated, washed with water, aqueous NaHCO3 and brine. The organic layer was dried (MgSO4) and concentrated. Purification of the residue by silica gel chromatography (eluting ethyl acetate/iso-hexane (1:3 to 1:1) gave the subtitle product (1.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06555541B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-79cb33d8ce114dfabbebb9cf883e5d9c |
| Source note | uspto-grants-2003_04 |