関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-methyl-N-(2,2,2-trifluoro-1-hydroxyethyl)benzamide | HCID 12150322 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(1-chloro-2,2,2-trifluoroethyl)-4-methylbenzamide | HCID 12150323 | 63.6% |
反応手順
A stirred solution of Example 1A (3.48 g, 15.0 mmol) in CH2Cl2 (60 mL) at 0° C. was treated with pyridine (1.20 mL). The reaction mixture was treated dropwise with thionyl chloride (1.10 mL, 15.0 mmol), and the reaction flask was equipped with a calcium chloride drying tube. The reaction mixture was stirred at 0° C. for 4 hours, the cooling bath was removed, and the solution was stirred at ambient temperature for an additional 12 hours. Concentration of the reaction mixture provided a white solid which was triturated with diethyl ether (2×200 mL) to provide 2.40 g of the desired product as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06645968B2 |
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| 出典データセット | uspto-grants-2003_11 |
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| ORD ID | ord-d28284691f8040318f5a67ad89dcfc2e |
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| 出典メモ | uspto-grants-2003_11 |
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