関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Di-tert-butyl Iminodicarboxylate | HCID 279800 | — |
| 反応物 | 3-(Bromomethyl)-6-phenylpyridazine | HCID 66717445 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-[Bis(tert-butoxycarbonyl)aminomethyl]-6-phenylpyridazine | HCID 66717700 | 97% |
反応手順
To a solution of 3-bromomethyl-6-phenylpyridazine (120 mg, 0.482 mmol) obtained in Reference Example 2-(a) in N,N-dimethylformamide (1.57 ml) were added di-tert-butyl iminodicarboxylate (127 mg, 0.585 mmol) and potassium carbonate (134 mg, 0.970 mmol), followed by stirring at 50° C. for 2 hours. After completion of the reaction, water was added to the reaction solution, followed by extraction with ethyl acetate. The separated organic layer was dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography (eluent; hexane:ethyl acetate=2:1→1:1 (V/V)), and fractions containing the desired compound were concentrated under reduced pressure to afford the title compound (180 mg) as a slightly yellow solid. (Yield: 97%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08685986B2 |
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| 出典データセット | uspto-grants-2014_04 |
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| ORD ID | ord-758a4a0eba134c9d8bef620388914d09 |
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| 出典メモ | uspto-grants-2014_04 |
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