関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl 3-(methylamino)but-2-enoate | HCID 2734182 | — |
| 反応物 | 2-Chloro-4-fluorobenzoyl chloride | HCID 2736546 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178483602 | HCID 178483602 | — |
反応手順
To a mixture of methyl 3-(methylamino)-2-butenoate (i.e. the product of Step A) (10.25 g, 79.43 mmol) and triethylamine (13.26 mL, 9.63 g, 95.31 mmol) in toluene (125 mL) at 0° C. was added dropwise 2-chloro-4-fluorobenzoyl chloride (15.25 g, 79.48 mol) in toluene (25 mL) over 30 minutes while maintaining the temperature of the reaction mixture between about 0 to 5° C. The reaction mixture was allowed to warm to room temperature and stirred over night. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The resulting dark yellow oil was triturated with hexanes and filtered to provide the title compound as a white solid (15.91 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08754115B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-c2780f1beab64aee9f3d1542d987565d |
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| 出典メモ | uspto-grants-2014_06 |
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