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Sodium hydride → Propane-1-sulfonic acid [2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-yl]-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Propanesulfonyl chloride | HCID 66279 | — |
| 反応物 | 6-(2,6-Dichlorophenyl)pyrido[2,3-d]pyrimidine-2,7-diamine | HCID 5328113 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Propane-1-sulfonic acid [2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-yl]-amide | HCID 53755885 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733913 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-587171f404ec4562b7f202a047a9a693 |
| 出典メモ | uspto-grants-1998_03 |