関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyryl chloride | HCID 8855 | — |
| 反応物 | Bay-H-1127 | HCID 16736 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-[5-(trifluoromethyl)-1H-indazol-3-yl]butanamide | HCID 10378475 | — |
反応手順
0.26 cm3 of butyryl chloride is added to 500 mg of 5-(trifluoromethyl)-1H-indazole-3-amine, prepared according to patent U.S. Pat. No. 3,133,081, in 15 cm3 of pyridine, and cooled to about 5° C. The reaction medium is allowed to return to about 19° C. over 12 hours. The reaction medium is evaporated under reduced pressure (2 kPa; 50° C.). The residue is taken up in 15 cm3 of ethyl acetate and 15 cm3 of distilled water. The organic phase is dried over magnesium sulphate, filtered through a sinter funnel and then evaporated under reduced pressure (2 kPa; 50° C.). The residue is taken up in 15 cm3 of dichloromethane, filtered and dried under reduced pressure (90 Pa; 50° C.) to give 390 mg of N-[5-(trifluoromethyl)-1H-indazol-3-yl]butanamide in the form of an off-white solid melting at 230° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06949579B2 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-beba78b9880f44de8bb9822551b1b2fb |
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| 出典メモ | uspto-grants-2005_09 |
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