関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trifluoroacetamidine | HCID 2776882 | — |
| 反応物 | Hexafluoro phosphate | HCID 6477909 | — |
| 反応物 | HCID 10590808 | HCID 10590808 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-Chloro-2-(trifluoromethyl)pyrimidine | HCID 33697960 | 56.2% |
反応手順
A solution of 4.70 g (85% purity, 35.65 mmol) of trifluoroacetamidine and 10.93 g (35.65 mmol) of ((Z)-2-chloro-3-dimethylamino-allylidene)-dimethyl-ammonium; hexafluoro phosphate [Davies, Ian W.; Marcoux, Jean-Francois; Wu, Jimmy; Palucki, Michael; Corley, Edward G.; Robbins, Michael A.; Tsou, Nancy, Ball, Richard G.; Dormer, Peter; Larsen, Robert D.; Reider, Paul J, Journal of Organic Chemistry 2000, 65(15), 4571-4574] in 70 ml acetonitrile was treated with 4.33 ml (42.78 mol) of triethylamine and stirred for 4 h at room temperature. The reaction was poured into 250 ml of water and extracted with ether (three times). The organic phases were washed with water (two times), dried (Na2SO4) and carefully evaporated to give 3.66 g of the title compound as an orange volatile liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07253192B2 |
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| 出典データセット | uspto-grants-2007_08 |
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| ORD ID | ord-7671513651e443afa296bc72042681e4 |
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| 出典メモ | uspto-grants-2007_08 |
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