関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diethyl methylmalonate | HCID 11857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Acetamide, N-(4-(chloromethyl)phenyl)- | HCID 148705 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Diethyl methyl-(4-acetamido)benzylmalonate | HCID 54008305 | — |
反応手順
Suspend sodium hydride (10.1 g, 0.21 mol) in tetrahydrofuran (300 mL), place under a nitrogen atmosphere and cool to 0° C. Add, by dropwise addition, diethyl methylmalonate (34.8 g, 0.2 mol). Stir for 30 minutes at 0° C. and add 4-acetamidobenzyl chloride (38.6 g, 0.21 mol). Heat at reflux for 5 hours, cool and pour into water (400 mL). Extract with ethyl acetate (3×600 mL), dry (MgSO4) and evaporate the solvent in vacuo to give diethyl methyl-(4-acetamido)benzylmalonate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05208240 |
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| 出典データセット | uspto-grants-1993_05 |
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| ORD ID | ord-b9fb229e404a4af4a10cf640f17b2088 |
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| 出典メモ | uspto-grants-1993_05 |
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