関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1,2,3,5-Tetrafluoro-4-nitrobenzene | HCID 67566 | — |
| 反応物 | 2-Fluoro-4-iodoaniline | HCID 185694 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,3,5-trifluoro-N-(2-fluoro-4-iodophenyl)-6-nitroaniline | HCID 57430072 | 59.24% |
反応手順
A stirred solution of 2-fluoro-4-iodoaniline (3.64 gm, 15.37 mmol) in dry THF (100 ml) under nitrogen was cooled to −78° C. and a solution of 1.0 M lithium hexa methyl disilazide (LiN(SiMe3)2) “LHMDS” (15.37 ml, 15.37 mmol) was added slowly. This reaction mixture was kept stirring at −78° C. for another hour and then 2,3,4,6-tetrafluoronitrobenzene was added. The reaction mixture was allowed to warm to room temperature and stirring continued for another 16 hours. Ethyl acetate (200 ml) was added to the reaction mixture and was washed with water. Organic layer was dried over sodium sulfate and further purified by column chromatography to provide yellow solid (3.75 gm, yield: 59.24%). M−H+: 410.9. 1H NMR (DMSO, 300 MHz): 6.85 (t, 1H); 7.38 (d, 1H); 7.62 (m, 2H); 8.78 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08648116B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-d3001c237f7e4fb6a70b29de9dd72c68 |
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| 出典メモ | uspto-grants-2014_02 |
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