関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 反応物 | HCID 178418310 | HCID 178418310 | — |
| 反応物 | HCID 178418314 | HCID 178418314 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-Butyl-tert-butylchlorophosphine | HCID 12625174 | — |
反応手順
To a solution of phosphorus trichloride (55 g) in dry diethyl ether (200 cm3) stirred and maintained at between -25° C. and -30° C. in an atmosphere of dry nitrogen, a 2 molar solution of tert-butyl magnesium chloride in diethyl ether (200 cm3, solution supplied by Aldrich Chemical Co.) was added during 45 min. After a further 15 min. a 2 molar solution of 2-butyl magnesium chloride (200 cm3, solution supplied by Aldrich Chemical Co.) was added in the same way. The suspension was stirred at -25° C. for a further 45 min., then allowed to reach ambient temperature, and finally boiled under reflux for 30 min., cooled, filtered to remove magnesium chloride, and distilled, yielding 2-butyl-tert-butylchlorophosphine (47 g), b.p. 74° C. under a pressure of 15 mm of mercury.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728853 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-f09ba275a47d468cb9ceb88c522a8f48 |
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| 出典メモ | uspto-grants-1998_03 |
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