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Ethanolamine → N-{6-[2-(5-Bromopyrimidin-2-yloxy)ethoxy]-2-(2-hydroxyethylamino)-5-(2-methoxyphenoxy)pyrimidin-4-yl}-4-tert-butylbenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanolamine | HCID 700 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | N-{6-[2-(5-bromopyrimidin-2-yloxy)ethoxy]-5-(2-methoxy-phenoxy)-2-methylsulfonylpyrimidin-4-yl}-4-tert-butylbenzenesulfonamide | HCID 10963585 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | N-{6-[2-(5-Bromopyrimidin-2-yloxy)ethoxy]-2-(2-hydroxyethylamino)-5-(2-methoxyphenoxy)pyrimidin-4-yl}-4-tert-butylbenzenesulfonamide | HCID 18931063 | 11.7% |
反応手順
A mixture of N-{6-[2-(5-bromopyrimidin-2-yloxy)ethoxy]-5-(2-methoxy-phenoxy)-2-methylsulfonylpyrimidin-4-yl}-4-tert-butylbenzenesulfonamide (500 mg), ethanolamine (172 mg) and dimethylacetamide (4 ml) is heated with stirring at 110°-120° C. for 20 hours. After cooling, to the mixture is added an aqueous ammonium chloride solution, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried, and evaporated under reduced pressure to remove the solvent. The residue is purified by silica gel column chromatography (solvent; chloroform:ethyl acetate=3:1) to give the title compound (57 mg) as a powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05739333 |
| 出典データセット | uspto-grants-1998_04 |
| ORD ID | ord-8d2df527486946448fdc9890de0fd748 |
| 出典メモ | uspto-grants-1998_04 |