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Dimethyl Carbonate → Methyl 2-(4-bromopyridin-2-yl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Carbonate | HCID 12021 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 反応物 | 4-Bromo-2-methylpyridine | HCID 2762835 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 2-(4-bromopyridin-2-yl)acetate | HCID 84071108 | — |
反応手順
To a mixture of 4-bromo-2-methylpyridine (1 g, 5.8 mmol) in 15 mL of anhydrous THF was added LDA (9.2 mL, 2M) dropwise at −70, stirred for 30 min dimethyl carbonate (630 mg, 7.0 mmol) was added dropwise to the above solution. After stirring for another 1 h, LC-MS found the reaction finished. It was quenched by Sat. NH4Cl solution and extracted with EtOAc. The organic layer was separated and evaporated under reduced pressure. The crude product was purified by a standard method to give desired product. LC-MS: m/z (M+H) 231.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029531B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-a47a24c68cc7420984d4030bc5703904 |
| 出典メモ | uspto-grants-2015_05 |