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

HRID 997

反応式

HRID 997 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-5441fae977e64216866214e130a2476a
出典データセット
uspto-grants-1998_03
特許番号
US05723409

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