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Triethylamine → HCID 178448490、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Chloro-2-methoxybenzoyl chloride | HCID 12384176 | — |
| 反応物 | 3-butyl-5-tert-butyl-1,3-thiazol-2(3H)-imine hydroiodide | HCID 66852177 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178448490 | HCID 178448490 | — |
反応手順
To a solution of Example 6A (1.4 g, ˜4 mmol) and triethylamine (1.4 mL, 10 mmol) in CH2Cl2 (35 mL) at 0° C. was added 5-chloro-2-methoxy-benzoyl chloride (820 mg, 4 mmol), the mixture was allowed to warm to room temperature was stirred for 14 hours. The mixture was washed sequentially with water, brine, dried with anhydrous MgSO4, filtered and concentrated under reduced pressure. The residue was purified by chromatography (6:2:2 Hexane-EtOAc-CH2Cl2) to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ: 0.94 (t, J=7 Hz, 3H), 1.30 (m+s, 11H), 1.75 (m, 2H), 3.77 (s, 3H), 4.14 (t, J=7 Hz, 2H), 7.10 (d, J=9 Hz, 1H), 7.31 (s, 1H), 7.43 (d-d, J=9 Hz, 3 Hz, 1H), 7.65 (d, J=3 Hz, 1H); MS (ESI+) m/z 381 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865753B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-b7585692fe684163a142c7b1c0b08f20 |
| 出典メモ | uspto-grants-2014_10 |