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Diethyl Malonate → Diethyl 2-(2-bromobenzyl)malonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | 2-Bromobenzyl bromide | HCID 76965 | — |
| 反応物 | Sodium Bromide | HCID 253881 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Diethyl 2-(2-bromobenzyl)malonate | HCID 12853296 | 71% |
反応手順
Diethyl malonate (77 g, 0.48 mol) was added to a stirred solution of sodium (10.2 g, 0.425 mol) in ethanol (800 ml) followed by 2-bromobenzyl bromide (100 g, 0.40 mol). Sodium bromide began to separate towards the end of the addition and the mixture became warm. The reaction was completed by refluxing on a steam bath for 3 hours and then cooling overnight. The bulk of the solvent was removed in vacuo, water was added and the product extracted into ether. After drying (CaCl2) and evaporation the product was distilled to give 93.28 g (71%) of material of bp0.2 130° C. (lit bp0.004 115°-120° C., F. G. Holliman and F. G. Mann J. Chem. Soc. 9, [1960]).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04699995 |
| 出典データセット | uspto-grants-1987_10 |
| ORD ID | ord-37e19e9937584beea98ab370d4bf0d4b |
| 出典メモ | uspto-grants-1987_10 |