関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | 1,1,3,3-Tetramethylguanidine | HCID 66460 | — |
| 反応物 | Ethyl 4,4,4-trifluorobut-2-enoate | HCID 141226 | — |
| 溶媒 | Ethyl Acetoacetate | HCID 8868 | — |
| 生成物 | Ethyl 4,4,4-trifluoro-3-(nitromethyl)butanoate | HCID 268363 | 81% |
反応手順
1.0 g (5.94 mmol) of 4,4,4-trifluoro-2-butenoic acid ethyl ester and 0.15 mL (1.19 mmol) of 1,1,3,3-tetramethyl guanidine and 1.6 mL (29.8 mmol) of nitromethane were mixed. The resulting mixture was cooled to 0° C. and then stirred for 3 hours at room temperature, followed by addition of 100 mL of ethylacetoacetate. The reaction mixture was washed with water, and then an organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give 1.1 g (4.80 mmol) of the title compound in a yield of 81%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07879848B2 |
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| 出典データセット | uspto-grants-2011_02 |
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| ORD ID | ord-ebabf3d7f64247c4a01f2fcabda03b19 |
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| 出典メモ | uspto-grants-2011_02 |
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