参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 二甲胺 | HCID 674 | — |
| 反应物 | methyl 2-(N-tert-butylsulfamoyl)-4-nitrobenzoate | HCID 15240542 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzenesulfonamide | HCID 15240543 | 76.8% |
反应步骤
115 g of N-tert.-butyl-2-methoxycarbonyl-5-nitro-benzenesulfonamide (Example c) in 1500 ml of methanol are gassed with about 200 g of dimethylamine. The mixture is stirred at about 35° C. for one week. The solution is concentrated under reduced pressure, the residue is taken up in ethyl acetate and the mixture is washed successively with dilute hydrochloric acid, saturated NaHCO3 solution and saturated NaCl solution. After drying over MgSO4, the organic phase is concentrated. 92 g of N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzensulfonamide are obtained: m.p.: 138-141° C.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US05922646 |
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| 来源数据集 | uspto-grants-1999_07 |
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| ORD ID | ord-acded5627ff04c47b809c9982851e0f7 |
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| 来源说明 | uspto-grants-1999_07 |
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