関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Carbonate | HCID 7766 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Benzyloxyphenylacetic acid ethyl ester | HCID 2737428 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Diethyl 2-(4-(benzyloxy)phenyl)malonate | HCID 2823246 | 78.9% |
反応手順
To a suspension of NaH (54 gm, 1.11 moles) in dry THF (500 ml) a solution of ethyl 2-(4-(benzyloxy)phenyl)acetate (100 gm, 0.37 moles) in dry THF (100 ml) was added at 0° C. To this was added diethyl carbonate (180 ml, 1.48 mole) dropwise over a period of one hour maintaining the reaction temperature at below 5° C. The reaction mixture was then stirred for 18 hours at 30° C. The contents of the reaction mixture were poured into ice cold water and extracted with ethyl acetate. The organic extract was successively washed with water & brine, dried over sodium sulfate and evaporated under reduced pressure to yield 100 gm of product as white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08772302B2 |
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| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-7d66fd5dc6d64dbd9bd789b81f8ed547 |
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| 出典メモ | uspto-grants-2014_07 |
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