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Pyridine → 4-Methyl-N-(1,2,2,2-tetrachloroethyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-methyl-N-(2,2,2-trichloro-1-hydroxyethyl)benzamide | HCID 3392664 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Methyl-N-(1,2,2,2-tetrachloroethyl)benzamide | HCID 12341576 | 89.2% |
反応手順
A stirred solution of Example 37C (20.0 g, 70.8 mmol) in CH2Cl2(300 mL) at 0° C. was treated with pyridine (10 mL). The reaction mixture was treated dropwise with thionyl chloride (10.4 mL, 141 mmol), and the reaction flask was equipped with a calcium chloride drying tube. The reaction mixture was warmed to ambient temperature and stirred for 4 hours. Concentration of the reaction mixture to a reduced volume and addition of diethyl ether (100 mL) resulted in a precipitate which was filtered off, and the filtrate was concentrated and dried under reduced pressure to provide 19.0 g of the desired product as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06645968B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-3714a12322254811b07426d335532996 |
| 出典メモ | uspto-grants-2003_11 |