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Pyridine → methyl 4-(N,N-dimethylsulfamoyl)amino-2-chlorobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dimethylsulphamoyl chloride | HCID 83372 | — |
| 反応物 | Methyl 4-Amino-2-chlorobenzoate | HCID 11839197 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | methyl 4-(N,N-dimethylsulfamoyl)amino-2-chlorobenzoate | HCID 22571711 | — |
反応手順
Pyridine (0.4 mL) was added to a solution of methyl 4-amino-2-chlorobenzoate (0.3 g) in CH2Cl2 (10 mL) at 0° C. under N2. N,N-Dimethylsulfamoyl chloride (0.21 mL) was added and the mixture was stirred at room temperature for 16 hours and refluxed for 5 hours. DMAP (0.4 g) was added and the mixture was stirred for 3 hours. The mixture was diluted with CH2Cl2 (100 mL), washed successively with 1N HCl, brine, satd. NaHCO3 and brine, dried and evaporated. The residue was purified by flash column chromatography (silica gel; eluent: EtOAc/hexane 1:3) to give 0.31 g of methyl 4-(N,N-dimethylsulfamoyl)amino-2-chlorobenzoate. ESMS: m/z 293 (MH+)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06855843B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-b4dc9b02a77c414a895c085f1167af81 |
| 出典メモ | uspto-grants-2005_02 |