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Acetic Acid → 2-(((1,1,1-Trifluoro-2-methylpropan-2-yl)amino)methylene)-succinonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | Succinonitrile | HCID 8062 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 1,1,1-Trifluoro-2-methylpropan-2-amine | HCID 11275188 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(((1,1,1-Trifluoro-2-methylpropan-2-yl)amino)methylene)-succinonitrile | HCID 90023004 | — |
反応手順
A solution of ethyl formate (330 mg, 4.46 mmol) and succinonitrile (300 mg, 3.75 mmol) in toluene (1561 μl) was added dropwise to a suspension of sodium methanolate (215 mg, 3.97 mmol) in toluene (1561 μl) at 0° C. After being stirred at RT for 3 h, the reaction mixture was treated with 1,1,1-trifluoro-2-methylpropan-2-amine (486 mg, 3.82 mmol) and acetic acid (255 μl, 4.46 mmol) then heated at 120° C. for 3 h. After being cooled to RT, the reaction mixture was washed with brine, then dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford the title compound as a brown oil, which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09303045B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-6830fa9bd52c4e4f868e2f2c20af2d0b |
| 出典メモ | uspto-grants-2016_04 |