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Potassium Carbonate → 5-Methoxy-2-(2-methoxy-2-oxoethoxy) benzoic acid, methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl bromoacetate | HCID 60984 | — |
| 反応物 | Methyl 2-hydroxy-5-methoxybenzoate | HCID 4072341 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Methoxy-2-(2-methoxy-2-oxoethoxy) benzoic acid, methyl ester | HCID 13961733 | 78% |
反応手順
A mixture of 50.0 g (0.27 mole) of 2-hydroxy-5-methoxybenzoic acid, methyl ester, 88.0 g (0.64 mole) of anhydrous potassium carbonate, and 25.4 ml (46.4 g, 0.30 mole) of methyl bromoacetate in 300 ml of N,N-dimethylformamide is stirred at room temperature for 24 hours. The reaction mixture is added to 1100 g of ice/water, stirred for 1 hour, and the precipitated crude product is filtered and washed with water. Recrystallization from aqueous methanol yields 54.7 g (78% yield) of analytically pure 5-methoxy-2-(2-methoxy-2-oxoethoxy) benzoic acid, methyl ester, mp 82°-85° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04703053 |
| 出典データセット | uspto-grants-1987_10 |
| ORD ID | ord-ccd8491cf69741ccadee6243ef224d2f |
| 出典メモ | uspto-grants-1987_10 |