HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 20261266, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 2-chloropyridine-3-sulfonamide | HCID 12234445 | — |
| Reactant | HCID 86740387 | HCID 86740387 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 20261266 | HCID 20261266 | 90% |
Reaction Steps
To a mixture of 0.652 g of 2-chloro-3-pyridinylsulfonamide and 0.55 ml of 1,8-diazabicyclo[5.4.0]undec-7-ene in 10 ml of absolute dioxan is added, at 25° C., 1 g of N-(4-difluoromethoxy-6-methylpyrimidin-2-yl)phenylcarbamate. The reaction mixture is stirred for another 2 hours at the same temperature and then concentrated. The residue is taken up in ice/water and neutralised with 1.86 ml of 2N hydrochloric acid. The precipitate is isolated, washed with water and dreid, affording 1.2 g (90%) of N-(2-chloro-3-pyridinylsulfonyl)-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)urea (compound 1.15) with a melting point of 161°-162° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04549898 |
| Source dataset | uspto-grants-1985_10 |
| ORD ID | ord-38af732e67a041199e279503d8ba113e |
| Source note | uspto-grants-1985_10 |