関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Menthol | HCID 1254 | — |
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Dichloro((1R,2S,5R)-2-isopropyl-5-methylcyclohexyloxy)phosphine | HCID 11054300 | 100% |
反応手順
The phosphorus trichloride (56.0 ml, 87.89 g, 0.640 mol) was added to dichloromethane (anhydrous) under argon gas to obtain a solution. The solution was cooled to −30° C. and (−)-menthol (1R,2S,5R) (10.00 g, 0.0640 mol) was added portion wise over 10 mins. The solution was allowed to warm to ambient temperature and was allowed to stir at ambient temperature for 16 hours. The solvent was removed in vacuo to obtain a colourless oil (16.46 g). The crude product was used directly in the subsequent step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08535655B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-418ec2ccf0174a49964151744e04de0f |
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| 出典メモ | uspto-grants-2013_09 |
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