二甲胺 → N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzenesulfonamide

HRID 581663

反应方程式

HRID 581663 反应方程式
[C:1]([NH:5][S:6]([C:9]1[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[CH:11][C:10]=1[C:18](OC)=[O:19])(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:22][NH:23][CH3:24]>CO>[C:1]([NH:5][S:6]([C:9]1[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[CH:11][C:10]=1[C:18]([N:23]([CH3:24])[CH3:22])=[O:19])(=[O:8])=[O:7])([CH3:2])([CH3:4])[CH3:3]

参与物

4

反应物 2

HCID 674二甲胺HCID 15240542methyl 2-(N-tert-butylsulfamoyl)-4-nitrobenzoate

产物 1

HCID 15240543N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzenesulfonamide收率 76.8%

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

反应条件

温度
35 °C

实验过程

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.

后处理

  1. concentrationThe solution is concentrated under reduced pressure
  2. washthe mixture is washed successively with dilute hydrochloric acid, saturated NaHCO3 solution and saturated NaCl solution
  3. dry with materialAfter drying over MgSO4
  4. concentrationthe organic phase is concentrated

来源与证据

ORD记录
ord-acded5627ff04c47b809c9982851e0f7
来源数据集
uspto-grants-1999_07
专利号
US05922646

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