HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosuccinimide → HCID 70579239, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 14570249 | HCID 14570249 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 70579239 | HCID 70579239 | — |
Reaction Steps
A mixture of 1'-methylxanthene-9-spiro-4'-piperidine hydrochloride (5 g.), N-chlorosuccinimide (4.5 g.) and dichloromethane (100 ml.) is refluxed for 72 hours. The solution is washed with saturated sodium bicarbonate solution then water and dried with MgS04. The solution is evaporated to give a gummy residue which is chromatographed on grade 3 aluminium oxide, Woelm basic. The product is eluted with 30% petroleum-ether (b.p. 60°-80° C.)/chloroform, taken up in ether and the solution treated with ethereal hydrochloric acid. The precipitate is filtered and recrystallised from ethanol-ether to give 2,7-dichloro-1'-methylxanthene-9-spiro-4'-piperidine hydrochloride, m.p. 285° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04001419 |
| Source dataset | uspto-grants-1977_01 |
| ORD ID | ord-c02a14a100ae4b90a748002859301f20 |
| Source note | uspto-grants-1977_01 |