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

HRID 581663

반응식

HRID 581663 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
35 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-acded5627ff04c47b809c9982851e0f7
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922646

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