HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68780053, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | N-1,2-Benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate | HCID 68778018 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68780053 | HCID 68780053 | 72% |
Reaction Steps
To a solution of N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) and triethylamine (0.309 ml, 2.22 mmol) in tetrahydrofuran (4 ml) was added benzyl chloroformate (0.120 ml, 0.833 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was poured to water and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of hexane and ethyl acetate to yield 152 mg (72.0%) of the desired product. mp 137-138° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07851473B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-d3883aef83844abca84321fe75b694bb |
| Source note | uspto-grants-2010_12 |