関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 7-[3,5-Difluoro-4-(2-propynyloxy)benzoyl]-7-azabicyclo[4.1.0]heptane | HCID 57701178 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | N-(2-chlorocyclohexyl)-3,5-difluoro-4-(2-propynyloxy)benzamide | HCID 57701136 | — |
反応手順
A mixture of 4 ml of chloroform and 298 mg of zinc (II) chloride was stirred at 60° C. After 5 minutes, a mixture of 291 mg of 7-[3,5-difluoro-4-(2-propynyloxy)benzoyl]-7-azabicyclo[4.1.0]heptane and 2 ml of chloroform was added dropwise thereto at 60° C., and the resulting mixture was heated under reflux for 5 hours. Then, an aqueous saturated ammonium chloride solution was added to the reaction mixture, and this was extracted with chloroform. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.22 g of N-(2-chlorocyclohexyl)-3,5-difluoro-4-(2-propynyloxy)benzamide (hereinafter, described as the compound 87 of the present invention) represented by the formula:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07902400B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-9c87c08183054d25addd37cb2ab63ce0 |
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| 出典メモ | uspto-grants-2011_03 |
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