HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → Propane-1-sulfonic acid [2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-yl]-amide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-Propanesulfonyl chloride | HCID 66279 | — |
| Reactant | 6-(2,6-Dichlorophenyl)pyrido[2,3-d]pyrimidine-2,7-diamine | HCID 5328113 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Propane-1-sulfonic acid [2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-yl]-amide | HCID 53755885 | — |
Reaction Steps
To a slurry of 1.00 g of 2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine from Example 1 in 15 mL of DMF was added 0.15 g sodium hydride (60% in mineral oil) portionwise and the mixture stirred for 1 hour. Propanesulfonyl chloride (0.39 mL) is added dropwise, and the reaction mixture stirred at ambient temperature for 16 hours. The reaction mixture is filtered to remove a small amount of insoluble material and the filtrate evaporated in vacuo. The product is purified by medium pressure liquid chromatography (MPLC) using silica gel and eluting with a gradient of CHCl3 :EtOAc (2:1) to CHCl3 :EtOAc (1:1) to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05733913 |
| Source dataset | uspto-grants-1998_03 |
| ORD ID | ord-587171f404ec4562b7f202a047a9a693 |
| Source note | uspto-grants-1998_03 |