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Iodine → bis(4-Fluorophenyl)methyl(5-iodo-1H-1,2,4-triazol-1-ylmethyl)silane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Flusilazole | HCID 73675 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | bis(4-Fluorophenyl)methyl(5-iodo-1H-1,2,4-triazol-1-ylmethyl)silane | HCID 14154944 | 18.8% |
反応手順
A solution of 3.14 g (0.010 mol) of bis(4-fluorophenyl)methyl(1H-1,2,4-triazol-1-ylmethyl)silane in 15 ml of THF was lithiated as described in Example 1, using 7.1 ml (0.011 mol) of 1.55M n-butyllithium in hexane. To this solution was added 1.4 g (0.011 mol) of iodine. The reaction mixture was allowed to warm to 0°, stirred 3 hours, poured into 1:1 ether/hexanes, washed with 7% aqueous NaHCO3 and brine, dried over Na2SO4, filtered and evaporated. The crude product was flash chromatographed (5% ether/methylene chloride) to give 0.83 g of the title compound as a white solid: m.p. 102°-104°; nmr (CDCl3) δ 0.7 (3H, s), 4.2 (2H, s), 7.1 (4H, m), 7.5 (4H, m), 7.8 (1H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04729986 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-7275c89fbcc84c8081509a78ed85e49b |
| 出典メモ | uspto-grants-1988_03 |