HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 23169248, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 10154328 | HCID 10154328 | — |
| Reactant | HCID 19814298 | HCID 19814298 | — |
| Solvent | Methyl Isobutyl Ketone | HCID 7909 | — |
| Product | HCID 23169248 | HCID 23169248 | 84.5% |
Reaction Steps
A mixture containing 7.3 g of 3-methyl-4-methylene-2-oxo-1-oxa-3,8-diazaspiro[4,5]decane, 9 ml of anhydrous triethylamine, 22.0 g of 3-(2-acetyl-10H-phenothiazin-10-yl)-propyl bromide and 80 ml of methyl isobutyl ketone is refluxed under argon while stirring for 6 hours. After cooling down the organic phase is washed with water, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The crude product obtained is purified by chromatography on a silica gel column by using first chloroform and then ethyl acetate as eluating agent. After combining the ethyl acetate eluate is evaporated under reduced pressure and the residue is recrystallized from ethanol to give the title compound in 84.5% yield, m.p.: 105°-106° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05157038 |
| Source dataset | uspto-grants-1992_10 |
| ORD ID | ord-bbcfbaac8d5843fc9d0fdb5702182674 |
| Source note | uspto-grants-1992_10 |