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Dimethylamine methanol → N-[5-chloro-2-(dimethylsulfamoyl)benzyl]acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine methanol | HCID 22497844 | — |
| 反応物 | 2-[(Acetylamino)methyl]-4-chlorobenzenesulfonyl chloride | HCID 86650829 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-[5-chloro-2-(dimethylsulfamoyl)benzyl]acetamide | HCID 66877112 | — |
反応手順
(Step 1) To a solution of 2N dimethylamine methanol solution (7.51 ml) in methanol (15 ml) was added dropwise a suspension of 2-[(acetylamino)methyl]-4-chlorobenzenesulfonyl chloride (2.12 g) in tetrahydrofuran (5 ml) under ice-cooling. The mixture was allowed to warm to room temperature, and stirred for 3 hr. The reaction mixture was quenched with water, and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to give N-[5-chloro-2-(dimethylsulfamoyl)benzyl]acetamide (1.77 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07985862B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-74ba9b8514fd47f9b611f683b5aeb474 |
| 出典メモ | uspto-grants-2011_07 |