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1-Naphthol → alpha-Naphthoxymalonic acid diethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Naphthol | HCID 7005 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Diethyl bromomalonate | HCID 69637 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | alpha-Naphthoxymalonic acid diethyl ester | HCID 54105534 | — |
反応手順
A solution of 25 g of 1-naphthol in 50 ml of DMF is slowly added dropwise to a solution of 7.6 g of sodium hydride dispersion in 300 ml of DMF. The suspension is stirred for 30 minutes and subsequently 41.5 g of bromomalonic acid diethyl ester in 50 ml of DMF are added dropwise. The reaction mixture is further stirred for 16 hours at room temperature and then concentrated by evaporation in a high vacuum. The residue is dissolved in ethyl acetate and washed with 2N sodium hydroxide solution, water and brine, dried over sodium sulphate and concentrated by evaporation. The residue is distilled at 145°-170°/2.6 Pa and yields α-naphthoxymalonic acid diethyl ester in the form of an orange-coloured oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727060 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-9f8a984e88484318932c00f0f1933f40 |
| 出典メモ | uspto-grants-1988_02 |