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Sulfuric Acid → Dimethyl pyridine-3,5-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 3,5-Pyridinedicarboxylic acid | HCID 10366 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Dimethyl pyridine-3,5-dicarboxylate | HCID 78339 | — |
反応手順
3,5-Pyridinedicarboxylic acid (1.5 g, 63 mmol) and conc. H2SO4 (0.9 mL) in MeOH (15 mL) are heated in a microwave oven at 120° C. for 2 h. The solvent is evaporated to give a residue with is partitioned between ethyl acetate and sat. aq. NaHCO3. The organic phase is washed with brine, dried over Na2SO4, filtered and evaporated to give a light yellow solid. MS (LC-MS): 196 [M+H]+ TLC, Rf (ethyl acetate/hexane 1:1)=0.56.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08129411B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-e396cb8fdfe14eef972433d8f391636a |
| 出典メモ | uspto-grants-2012_03 |