関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4,6-dichloro-N-ethylpyrimidin-2-amine | HCID 6493735 | — |
| 反応物 | N-(4-sulfamoyl-phenyl)-acetamide potassium salt | HCID 70262342 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | N-[4-(6-chloro-2-ethylamino-pyrimidin-4-ylsulfamoyl)-phenyl]-acetamide | HCID 10809139 | 75% |
反応手順
2.0 g (0.011 mol) of (4,6-dichloropyrimidin-2-yl)-ethylamine and 5.67 g (0.022 mol) of N-(4-sulfamoyl-phenyl)-acetamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone at 140° C. for 8 hours. Then, the solvent was distilled off in a high vacuum, the residue was partitioned in ethyl acetate/water, the inorganic phase was saturated with sodium chloride and the residual ethyl acetate dissolved in the aqueous phase was distilled off on a rotary evaporator. The aqueous phase was made acid with 1N HCl, the crystals which separated were filtered off under suction and washed with water. After drying there were obtained 2.88 g (75%) of N-[4-(6-chloro-2-ethylamino-pyrimidin-4-ylsulfamoyl)-phenyl]-acetamide as beige crystals, which were used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06030976 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-fe9e5b72d9ee4d6abb2c563cd596b606 |
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| 出典メモ | uspto-grants-2000_02 |
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