関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diphenylphosphinic chloride | HCID 73910 | — |
| 反応物 | (S,E)-8-(tert-Butyldiphenylsilyloxy)-2-methyloct-5-en-4-amine hydrochloride | HCID 53248329 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (S,E)-N-(8-(tert-Butyldiphenylsilyloxy)-2-methyloct-5-en-4-yl)-P,P-diphenylphosphinic amide | HCID 67310501 | 119.6% |
反応手順
To a solution of the amine 7 (400 mg, 1.01 mmol) in dry DCM (7 mL) were added Et3N (0.44 mL, 3.13 mmol), and then a solution of diphenylphosphinic chloride (Ph2POCl, 0.22 mL, 1.11 mmol) in dry DCM (3 mL) at 0° C. After being stirred at 0° C. for 15 min, the reaction mixture was allowed to warm to rt and stirred for 4 h, then diluted with DCM and 10% HCl. The aqueous phase was extracted with DCM and the combined organic layers were washed with sat. NaHCO3, dried (MgSO4), filtered and concentrated in vacuo to afford 720 mg of the crude title compound as a pale yellow solidified oil, which was used for the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822541B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-910e0a0fb494480ba9a21eaf7ef1f39a |
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| 出典メモ | uspto-grants-2014_09 |
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