HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Iodide → HCID 21428904, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | 1-Phenyl-1,3,8-triazaspiro(4.5)decan-4-one | HCID 70556 | — |
| Reactant | HCID 21428903 | HCID 21428903 | — |
| Solvent | Methyl Isobutyl Ketone | HCID 7909 | — |
| Product | HCID 21428904 | HCID 21428904 | — |
Reaction Steps
A mixture of 4.4 parts of N-(2-chloroethyl)-2-pyridinecarboxamide, 13.8 parts of 1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one, 3.3 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 24 hours. The reaction mixture is evaporated and the residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is converted into the hydrochloride salt in 2-propanol. The salt is filtered off and crystallized from ethanol, yielding 1.1 parts of N-[2-(4-oxo-1-phenyl-1,3,8-triazaspiro[4,5]dec-8-yl)ethyl]-2-pyridinecarboxamide dihydrochloride hydrate; mp. 250.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04031226 |
| Source dataset | uspto-grants-1977_06 |
| ORD ID | ord-219e6cd173e5461389feba78b0664820 |
| Source note | uspto-grants-1977_06 |