HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chlorophenol → 4-(4-Chlorophenoxy)-1-[3-(6-fluoro-1,2-benzisoxazol-3-yl)propyl]-piperidine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chlorophenol | HCID 4684 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | 1-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-4-hydroxypiperidine | HCID 13319866 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | 4-(4-Chlorophenoxy)-1-[3-(6-fluoro-1,2-benzisoxazol-3-yl)propyl]-piperidine hydrochloride | HCID 13319868 | 61.8% |
Reaction Steps
To a solution of 9.5 g of 1-[3-(6-fluoro-1,2-benzisoxazol-3-yl)-propyl]-4-hydroxypiperidine, 4.5 g of 4-chlorophenol and 9.8 g triphenylphosphine in 250 ml of benzene, cooled with an ice-bath, was slowly added over one hour a solution of 6.4 g of diethyl azodicarboxylate in 60 ml of benzene. After stirring one hr at ambient temperature, the reaction mixture was filtered and then concentrated to an oil. The oil was treated with ethereal hydrogen chloride to give 4.6 g (32%) of product, mp 209°-211° C. Recrystallization from ethyl acetate/methanol gave the analytical sample, mp 212°-213° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04591586 |
| Source dataset | uspto-grants-1986_05 |
| ORD ID | ord-1723d82be68848f695b653db700b60cd |
| Source note | uspto-grants-1986_05 |