HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 18931391, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| Reactant | HCID 18931229 | HCID 18931229 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18931391 | HCID 18931391 | 29% |
Reaction Steps
A mixture of 4-amino-1-[5-(5-chloro-2-methoxyphenyl)-5-oxopentyl]-piperidine-4-carboxamide (0.36 g, 1 mmol), prepared as in Example 21, 1,1'-thiocarbonyldiimidazole (0.23 g, 1.3 mmol), and DMF (3 mL) was heated 5 hours at 50°-60° C. and then diluted with water. The mixture was extracted with ethyl acetate and the extract was dried (MgSO4) and concentrated. The residue was purified by column chromatography eluting with methylene chloride/methanol+ammonium hydroxide (95:5) to give 8-[5-(5-chloro-2-methoxyphenyl)-5-oxopentyl]-2-thioxo-1,3,8-triazaspiro[4.5]decane-4-one (0.12 g, 0.29 mmol), m.p. 152°-154° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05739336 |
| Source dataset | uspto-grants-1998_04 |
| ORD ID | ord-9df70334b30e4d6f9c7d5723c02a81d1 |
| Source note | uspto-grants-1998_04 |