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Water → 1-[2-(4-{2-[(e)-2-(-4-Trifluoromethanesulfinyl-phenyl)-vinyl]-oxazol-4-ylmethoxy}-phenyl-methoxy)-ethyl]-1h-[1,2,3]triazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 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 | 4-Chloromethyl-2-[2-(4-trifluoromethylsulfinyl-phenyl)-vinyl]-oxazole | HCID 69292389 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[2-(4-{2-[(e)-2-(-4-Trifluoromethanesulfinyl-phenyl)-vinyl]-oxazol-4-ylmethoxy}-phenyl-methoxy)-ethyl]-1h-[1,2,3]triazole | HCID 11409778 | 31% |
反応手順
13.0 mg (0.50 mmol) 95% sodium hydride were given to a solution of 110 mg (0.50 mmol) 4-(2-[1,2,3]triazol-1-yl-ethoxymethyl)-phenol in 4.0 ml DMF and stirred for 15 min. 168 mg (0.50 mmol) 4-chloromethyl-2-[2-(4-trifluoromethanesulfinyl-phenyl)-vinyl]-oxazole were added and stirring continued at r.t. overnight. After addition of 10 ml water the resulting precipitate was washed twice with 10 ml water, 2×10 ml methanol/water 1:1 and with diethyl ether. The residue was purified by chromatography on silica gel (eluent: ethyl acetate/n-heptane 3:1) to yield 80 mg (31%) colorless powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07405231B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-b48cb373ed144cc98111a45c91931d62 |
| 出典メモ | uspto-grants-2008_07 |