関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 3,5-Bis(phenylmethoxy)benzoic acid | HCID 99307 | — |
| 反応物 | HCID 178418348 | HCID 178418348 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Ethanone, 1-(3,5-bis(phenylmethoxy)phenyl)- | HCID 120098 | — |
反応手順
Over a period of 1.5 hours, methyl lithium (531 ml. of a 2 molar solution, 1.06 M) is added under a nitrogen atmosphere to a rapidly stirring solution of 3,5-dibenzyloxybenzoic acid (175 g., 0.532 M) in ether (250 ml.)-tetrahydrofuran (1400 ml.) maintained at 15°-20° C. After stirring an additional 0.75 hour at 10°-15° C., water (600 ml.) is slowly added keeping the reaction temperature below 20° C. The aqueous layer is separated and extracted with ether (3×250 ml.). The organic phases are combined, washed with saturated sodium chloride solution (4×300 ml.), dried over sodium sulfate, and concentrated under vacuum to give an oil which slowly crystallized from isopropyl ether. The crude product is recrystallized from ether-hexane to yield 104.7 g. (59%) of product; m.p. 59°-61° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04400385 |
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| 出典データセット | uspto-grants-1983_08 |
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| ORD ID | ord-6e1c4bb4b50a4db28c3a94907d0c70c6 |
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| 出典メモ | uspto-grants-1983_08 |
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