HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylsulphamoyl chloride → Piperazine-1,4-disulfonic acid [2-(2,3-difluoro-benzylsulfanyl)-6-methoxy-pyrimidin-4-yl]-amide dimethylamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Reactant | N-[2-[[(2,3-Difluorophenyl)methyl]thio]-6-methoxypyrimidin-4-yl]piperazine-1-sulfonamide, trifluoroacetate salt | HCID 67051309 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Piperazine-1,4-disulfonic acid [2-(2,3-difluoro-benzylsulfanyl)-6-methoxy-pyrimidin-4-yl]-amide dimethylamide | HCID 59558811 | — |
Reaction Steps
The title compound was prepared by adding dimethyl sulfamoyl chloride to a solution of N-[2-[[(2,3-Difluorophenyl)methyl]thio]-6-methoxypyrimidin-4-yl]piperazine-1-sulfonamide, trifluoroacetate salt (the product from example 36) (0.25 g) in DCM (5 mL). Purification was by reverse phase HPLC (symmetry as the stationary phase and TFA/acetonitrile as the mobile phase) then titurated with Toluene, DCM followed by Et2O to give the title compound as a white solid. Yield: 0.11 g
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410123B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-3433c9335e474dc29d6af7f3bb9aadd7 |
| Source note | uspto-grants-2013_04 |