Dimethylamine → N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzenesulfonamide

HRID 581663

反応式

HRID 581663 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
35 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-acded5627ff04c47b809c9982851e0f7
出典データセット
uspto-grants-1999_07
特許番号
US05922646

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