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Sodium Cyanide → 4-Methylpyrimidine-2-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | 2-Chloro-4-methylpyrimidine | HCID 11629607 | — |
| 溶媒 | Trimethylamine | HCID 1146 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-Methylpyrimidine-2-carbonitrile | HCID 12684324 | 64.9% |
反応手順
To a solution of 2-chloro-4-methylpyrimidine (3.00 g, 23.3 mmol; 3B Pharmachem International, China) in ethyl ether (24 mL) was added a solution of sodium cyanide (2.86 g, 58.3 mmol) in trimethylamine solution (1:3, trimethylamine:water, 24.0 mL). The reaction mixture was stirred at room temperature overnight. The aqueous layer was extracted with ethyl ether (3×20 mL). The combined organic layers were dried over MgSO4, filtered, and concentrated under reduced pressure to yield the title compound, 4-methyl-pyrimidine-2-carbonitrile (1.80 g; 64.8%), which was used in the next step without further purification. 1H NMR (400 MHz, D2O) δ 8.64 (d, J=5.4 Hz, 1H), 7.59 (d, J=5.5 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198275B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-11577d72cb8e47d390396c7b1d4ba5e1 |
| 出典メモ | uspto-grants-2012_06 |