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Sodium hydride → 2,2,3,3-Tetramethylcyclopropanecarboxylic acid (5-chloro-3-(2-methoxy-ethy)-4-methyl-3H-thiazol-2-ylidene]-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Bromoethyl methyl ether | HCID 80972 | — |
| 反応物 | 2,2,3,3-Tetramethylcyclopropanecarboxylic acid (5-chloro-4-methyl-thiazol-2-yl)-amide | HCID 86618906 | — |
| 溶媒 | tetrahydrofuran N,N-dimethylformamide | HCID 21974620 | — |
| 生成物 | 2,2,3,3-Tetramethylcyclopropanecarboxylic acid (5-chloro-3-(2-methoxy-ethy)-4-methyl-3H-thiazol-2-ylidene]-amide | HCID 68621427 | — |
反応手順
A mixture of the product of Example 118A (150 mg, 0.55 mmol), NaH (60% dispersion in mineral oil, 29.0 mg, 0.71 mmol) and 2-bromoethyl methyl ether (57 μl, 0.61 mmol) in 20 mL of 2:1 THF/DMF was processed according to the method desribed in Example 112B to provide the title compound: 1H NMR (300 MHz, DMSO-d6) δ 1.18 (s, 6H) 1.23 (s, 6H) 1.50 (s, 1H) 2.29 (s, 3H) 3.25 (s, 3H) 3.63 (t, J=5.3 Hz, 2H) 4.27 (t, J=5.3 Hz, 2H); MS (DCI/NH3) m/z 331 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841334B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-7013e796aabd4f98a1fb27961d3ca491 |
| 出典メモ | uspto-grants-2014_09 |