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Sodium hydride → 1-[2-(4-{2-[2-(E)-(4-chloro-2-fluoro-phenyl)-vinyl]-oxazol-4-ylmethoxy}-benzyloxy)-ethyl]-1H-[1,2,3]triazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-(2-[1,2,3]Triazol-1-yl-ethoxymethyl)-phenol | HCID 21075895 | — |
| 反応物 | 2-[2-(4-Chloro-2-fluoro-phenyl)-vinyl]-4-chloromethyl-oxazole | HCID 69112985 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[2-(4-{2-[2-(E)-(4-chloro-2-fluoro-phenyl)-vinyl]-oxazol-4-ylmethoxy}-benzyloxy)-ethyl]-1H-[1,2,3]triazole | HCID 11626649 | 54% |
反応手順
380 mg (15 mmol) of 95% sodium hydride were given to a solution of 3.00 g (13.7 mmol) 4-(2-[1,2,3]triazol-1-yl-ethoxymethyl)-phenol in 70 ml N,N-dimethylformamide and stirred for 30 min at room temperature. Then 3.73 g (13.7 mmol) 2-[2-(4-chloro-2-fluoro-phenyl)-vinyl]-4-chloromethyl-oxazole were added and stirring continued over night. The mixture was quenched with water, stirred for 1 h and the precipitate isolated by filtration. After washing with water, little methanol, ethyl acetate/heptane 2:1 and ether, and drying at 40° C. in vacuo, 3.34 g (54%) 1-[2-(4-{2-[2-(E)-(4-chloro-2-fluoro-phenyl)-vinyl]-oxazol-4-ylmethoxy}-benzyloxy)-ethyl]-1H-[1,2,3]triazole were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07163953B2 |
| 出典データセット | uspto-grants-2007_01 |
| ORD ID | ord-19e2e3e6616a4f5c800abdb9bb011ccf |
| 出典メモ | uspto-grants-2007_01 |