HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 13076432, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Phenyl chloroformate | HCID 15891 | — |
| Reactant | HCID 13076414 | HCID 13076414 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 13076432 | HCID 13076432 | 65% |
Reaction Steps
A mixture of 1.74 g of 4-fluoro-3-(1-methyl-4-piperidyl)-1,2-benzisoxazole, 1.25 g of potassium carbonate, 1.40 g of phenyl chloroformate and 50.0 ml of toluene was stirred under reflux for 8.0 hrs. The mixture was poured into water and the toluene layer was separated, dried over anhydrous magnesium sulfate and the solvent was removed in vacuo to yield an oil. The oil was purified by passing through a silica gel column (20:1), using 1% methanol in dichloromethane as the eluent. The eluent was evaporated and the residue solidified when scratched to yield a solid. The solid was recrystallized from petroleum-ether (bp 30°-60°) to yield 1.6 g (65%) of product, mp 108°-110°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04528376 |
| Source dataset | uspto-grants-1985_07 |
| ORD ID | ord-7eb1d344781e48979e89b89cab4fcd41 |
| Source note | uspto-grants-1985_07 |