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Ethyl isocyanatoacetate → N-(3-aminosulfonyl-4-chloro-2-hydroxyphenyl)-N'-(ethoxycarbonyl)methylurea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl isocyanatoacetate | HCID 76283 | — |
| 反応物 | 3-Amino-6-chloro-2-hydroxy-benzenesulfonamide | HCID 11368059 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(3-aminosulfonyl-4-chloro-2-hydroxyphenyl)-N'-(ethoxycarbonyl)methylurea | HCID 10154964 | 7.5% |
反応手順
A solution of 3-amino-6-chloro-2-hydroxybenzenesulfonamide (170 mg, 0.76 mmol) and ethyl isocyanatoacetate (103 μL, 0.92 mmol) in 1.5 mL of N,N-dimethyl-formamide was stirred at room temperature for 20 hours. The mixture was diluted with ethyl acetate and washed with water to give the crude. Purification upon column chromatograph on silica gel, eluting with ethyl acetate/hexane (60/40, v/v), followed by Gilson HPLC separation, gave the desired product (20 mg, 7%). LC-MS (m/z) 352.0 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06767922B2 |
| 出典データセット | uspto-grants-2004_07 |
| ORD ID | ord-f2518a3388a049b690f3d2beba0e13ec |
| 出典メモ | uspto-grants-2004_07 |