関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl)acetate | HCID 67959054 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(4,6-Dimethoxypyrimidine-2-yl)acetonitrile | HCID 14580674 | — |
反応手順
Into a 50-ml eggplant-shaped flask provided with a magnetic stirrer and a reflux condenser were added 2.79 g (10 mmol) of tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl)acetate, 10 ml of toluene and then 0.38 g (4 mmol) of methanesulfonic acid. The system inside was purged with nitrogen and stirred for 2 hours at 100° C. After the completion of a reaction, the system was cooled to room temperature; 30 ml water and 30 ml of ethyl acetate were added for phase separation; and re-extraction was conducted using 20 ml of ethyl acetate. Two ethyl acetate phases were combined, washed with saturated sodium chloride water, and dried over anhydrous sodium sulfate. Then, ethyl acetate was distilled off under reduced pressure to obtain 2-cyanomethyl-4,6-dimethoxypyrimidine as white crystal of 1.45 g. HPLC purity: 95.7% Yield: 81%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08748605B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-15eeb50f2eed4a75bef0a3fed91f25b9 |
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| 出典メモ | uspto-grants-2014_06 |
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