HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 85927953, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methanesulfonamide | HCID 72879 | — |
| Reactant | Pyrimidine, 4,6-dichloro-2-[(phenylmethyl)thio]- | HCID 470488 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 85927953 | HCID 85927953 | — |
Reaction Steps
To methane sulphonamide (1.47 g) in DMF (30 ml) was added 60% sodium hydride (0.59 g) at room temperature and stirred for 1 h. To this mixture was then added the subtitle product of step ii) and the mixture stirred at room temperature for 6 h. To the reaction mixture was added EtOAc (50 ml) and aqueous hydrochloric acid (50 ml, 1M). The organic layer was separated and washed with brine (20 ml), combined, dried (MgSO4) and evaporated to dryness under reduced pressure. The residue was purified by column chromatography (20 to 50% EtOAc/iso-hexane) to afford the subtitle compound as a yellow oil. Yield: 1.60 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07582644B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-7a6241f770ec4ff08be0292ede4ea167 |
| Source note | uspto-grants-2009_09 |