関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Zinc | HCID 23994 | — |
| 反応物 | Ethyl Nonanoate | HCID 31251 | — |
| 反応物 | Disodium acetylide | HCID 560317 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | HCID 178471365 | HCID 178471365 | — |
反応手順
In a dry reaction tube under nitrogen were charged zinc dust (3.70 g, 56.6 mmol), iodine (479 mg, 1.89 mmol) and dry DMA (20 mL). The mixture was stirred at room temperature until the color of iodine disappeared. Ethyl 9-bromononanoate was added, and the mixture was stirred at 80° C. for 4 hours and then at room temperature overnight. (Completion of the zinc insertion reaction was checked by GCMS analysis of the hydrolyzed reaction mixture.) The reaction mixture was used without further treatment in the subsequent step. GCMS m/z 186 [M]+ (ethyl nonanoate).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09393315B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-0ef785149a124889a3ddb5d4f53c3659 |
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| 出典メモ | uspto-grants-2016_07 |
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