関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Bromo-2-methylpropane | HCID 6555 | — |
| 反応物 | 2-tert-Butyl-1,1,3,3-tetramethylguanidine | HCID 3571581 | — |
| 反応物 | N-(5-isopropylpyridin-2-yl)-4-vinylbenzenesulfonamide | HCID 89876040 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-isobutyl-N-(5-isopropylpyridin-2-yl)-4-vinylbenzenesulfonamide | HCID 89875813 | — |
反応手順
To a solution of N-(5-isopropylpyridin-2-yl)-4-vinylbenzenesulfonamide (507 mg, 1.677 mmol) in acetonitrile (10 mL), was added 2-(tert-butyl)-1,1,3,3-tetramethylguanidine (0.676 mL, 3.35 mmol). The mixture was stirred at room temperature for 1 hour, then 1-bromo-2-methylpropane (0.676 mL, 3.35 mmol) added. The reaction was then heated by microwaves to 150° C., for 30 minutes. After cooling, the solvent was removed under a stream of nitrogen and the crude purified by normal phase chromatography on silica (Si) (0-50% ethyl acetate-cyclohexane gradient). The appropriate fractions were combined and evaporated in vacuo to give the title product, 179 mg, as a yellow oil which solidified on standing. LCMS (2 min, High pH) Rt 1.49 min, m/z (ES+) 359 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09242972B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-b0067cfcdbfa4507a5b4380cd84530c2 |
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| 出典メモ | uspto-grants-2016_01 |
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