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Tetrahydrofuran → rac-4-(1-Hydroxyethyl)-N-methylpyridine-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-formyl-N-methylpicolinamide | HCID 21963889 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | rac-4-(1-Hydroxyethyl)-N-methylpyridine-2-carboxamide | HCID 68047396 | — |
反応手順
At 0° C. and under argon, 393 mg (2.394 mmol) of 4-formyl-N-methylpyridine-2-carboxamide Example 42A were initially charged in 66 ml abs. tetrahydrofuran. At 0° C., 343 mg (2.873 mmol) of methylmagnesium bromide [1.4 mol in toluene/tetrahydrofuran 3/1] were added dropwise, and the reaction solution was stirred at this temperature for 1 h. 200 μl of semisaturated aqueous sodium bicarbonate solution and 200 ml of ethyl acetate were added to the reaction solution. The precipitate was filtered off and washed with ethyl acetate. The filtrate was evaporated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09187428B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-825df3cf2f284e63927ca94387325f65 |
| 出典メモ | uspto-grants-2015_11 |