methyl 2-(N-tert-butylsulfamoyl)-4-nitrobenzoate → methyl 4-amino-2-(N-tert-butylsulfamoyl)benzoate

HRID 997

反应方程式

HRID 997 反应方程式
[C:1]([NH:5][S:6]([C:9]1[CH:14]=[C:13]([N+:15]([O-])=O)[CH:12]=[CH:11][C:10]=1[C:18]([O:20][CH3:21])=[O:19])(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2].[H][H]>CO>[C:1]([NH:5][S:6]([C:9]1[CH:14]=[C:13]([NH2:15])[CH:12]=[CH:11][C:10]=1[C:18]([O:20][CH3:21])=[O:19])(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2]

参与物

4

反应物 2

HCID 15240542methyl 2-(N-tert-butylsulfamoyl)-4-nitrobenzoateHCID 178418361HCID 178418361，化合物

产物 1

HCID 10946074methyl 4-amino-2-(N-tert-butylsulfamoyl)benzoate

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

实验过程

25.08 g (0.079 mol) of N-tert-butyl-2-methoxycarbonyl-5-nitrobenzenesulfonamide are dissolved in 1000 ml of MeOH. 0.50 g of Pd--C (10%) is added and the mixture is shaken under a hydrogen atmosphere (1 atm) until the uptake of hydrogen has finished. The catalyst is separated off and the solvent is removed by distillation. The residue is induced to crystallize by stirring with a little ethyl acetate. The resulting N-tert-butyl-5-amino-2-methoxycarbonylbenzenesulfonamide (18.3 g; 80.9% of theory) melts at 193° C.

后处理

  1. customThe catalyst is separated off
  2. customthe solvent is removed by distillation
  3. customto crystallize

来源与证据

ORD记录
ord-5441fae977e64216866214e130a2476a
来源数据集
uspto-grants-1998_03
专利号
US05723409

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