関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trichloroacetonitrile | HCID 11011 | — |
| 反応物 | 2,4-Difluorobenzyl alcohol | HCID 91867 | — |
| 触媒 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Potassium Hydroxide | HCID 14797 | — |
| 生成物 | 2,4-Difluorobenzyl trichloroacetimidate | HCID 11077074 | 92% |
反応手順
Tetrabutyl ammonium hydrogen sulphate (15 mg) was added to 2,4-difluorobenzylalcohol (1.0 g, 6.94 mmol) in CH2Cl2 (10 ml) and KOH (50%, 10 ml). This mixture was cooled to −15° C. prior to the addition of trichloroacetonitrile (1.2 ml, 8.32 mmol). After 30 min at −15° C. and 3 h at ambient temperature the phases were separated. The aqueous phase was extracted twice with CH2Cl2. The combined organic phases were dried with MgSO4 and reduced to one third. The residue was filtered through celite and concentrated to give the crude 2,4-difluorobenzyl trichloroacetimidate (1.83 g, 92%) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06489364B2 |
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| 出典データセット | uspto-grants-2002_12 |
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| ORD ID | ord-28cd121bda794ab8b9cb5eef5712f152 |
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| 出典メモ | uspto-grants-2002_12 |
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