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Dimethylformamide → Methyl 2-methoxy-3-methylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 3-Methylsalicylic Acid | HCID 6738 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 生成物 | Methyl 2-methoxy-3-methylbenzoate | HCID 13229229 | 59.3% |
反応手順
199.9 g (1.45 mol) of potassium carbonate is introduced into 1.5 1 of dimethylformamide. At room temperature, 100 g (657.29 mol) of 2-hydroxy-3-methylbenzoic acid, dissolved in 250 ml of dimethylformamide, is added in drops. After 30 minutes of stirring, 90 ml of methyl iodide is added in drops, and the batch is stirred overnight. The reaction mixture is added to ice water and extracted three times with methyl tert-butyl ether. The organic phases are washed with water and brine. After drying, the solvent is spun off, and the residue is chromatographed on silica gel (mobile solvent ethyl acetate/hexane). 70.21 g (59.3%) of the desired compound is isolated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07638515B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-e592de29152a4a62af76d0ee6855aa9e |
| 出典メモ | uspto-grants-2009_12 |