HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 19377398, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl ester | HCID 10945667 | — |
| Reactant | 3-[1-(Acetyloxy)-2-fluoroethyl]-2-pyridinesulfonamide | HCID 19377413 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 19377398 | HCID 19377398 | 89% |
Reaction Steps
To 4.1 g of 3-(1-acetoxy-2-fluoroethyl)-2-pyridinesulfonamide in 50 ml of acetonitrile is added 4.22 g of phenyl(4,6-dimethoxypyrimidin-2-yl)carbamate and 2.4 g of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). After stirring at room temperature for 2 hours the solution is acidified to pH 4.5 with 5% hydrochloric acid. The resultant solution is extracted with methylene chloride and the methylene chloride phase is dried over magnesium sulfate, filtered and evaporated. Trituration of the residue with Et2O yields 6 g of the product (solid, Yield: 89%), which is washed with a mixture solvent of ethylacetate/n-hexane(1/1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05461026 |
| Source dataset | uspto-grants-1995_10 |
| ORD ID | ord-90a921a63a7d48ba8c5ebcdbe5c5d637 |
| Source note | uspto-grants-1995_10 |