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Water → Methyl 2-chloronicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Chloronicotinic acid | HCID 76258 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 2-chloronicotinate | HCID 819931 | 40% |
反応手順
A solution of 2-chloronicotinic acid (1.61 g, 10.2 mmol) and sulfuric acid (0.5 mL) in methanol (30 mL) was stirred at reflux overnight. The solution was poured into water (100 mL) and neutralised with NaHCO3 (s) before being extracted with 1:1 hexane/ethyl acetate (3×40 mL). The solvents were dried (MgSO4) and evaporated and the residue was purified by flash column chromatography (SiO2, 25% ethyl acetate/hexane eluent) to afford the ester as a colourless oil (700 mg, 40%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07381734B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-54e1d1195258426687008a009f96fe02 |
| 出典メモ | uspto-grants-2008_06 |