HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 18365062, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 18365072 | HCID 18365072 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 18365062 | HCID 18365062 | 152.3% |
Reaction Steps
A solution of ethyl 3′,4′-dihydro-4′-oxospiro[piperidine-4,2′-[1′H]-(pyrido[2,3-d]-pyrimidine)]-1-carboxylate (0.74 g, 2.55 mmol) and Lawesson's reagent (0.62 g, 1.5 mmol) in dioxane (15 ml) was heated at reflux for 2 h. The mixture was absorbed onto silica gel and purified by flash column chromatography on silica gel, eluting with dichloromethane/methanol (50:1) to afford the product as a white solid (0.7 g). MS (+CI) m/Z 307 [M+H]+; 1H NMR (d6-DMSO) 10.37 (1H, dd), 8.34 (1H, dd), 8.24 (1H, dd), 8.10 (H, s), 6.76 (1H, dd), 4.04 (2H, q), 3.6-3.78 (2H, m), 3.3-3.5 (2H, m), 1.75-1.90 (4H, m), 1.21 (3H, t).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06303613B1 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-1232e07e0f3a4a2a84b3e846caee62be |
| Source note | uspto-grants-2001_10 |