Hydrochloric Acid → 3-Amino-N,N-diethylbenzene-1-sulfonamide

HRID 1110673노트

반응식

HRID 1110673 반응식
[CH2:1]([N:3]([CH2:16][CH3:17])[S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-])=O)[CH:8]=1)(=[O:6])=[O:5])[CH3:2].Cl>CO>[CH2:16]([N:3]([CH2:1][CH3:2])[S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([NH2:13])[CH:8]=1)(=[O:6])=[O:5])[CH3:17]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 232031N,N-Diethyl-3-nitrobenzenesulfonamide

생성물 1

HCID 29635153-Amino-N,N-diethylbenzene-1-sulfonamide수율 87%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The N,N-diethyl-3-(nitro)benzenesulfonamide (3.9 g) was dissolved in methanol (60 ml) and, after an addition of conc. hydrochloric acid (10 ml), reduced iron (4.2 g) was added and the mixture was stirred at room temperature for 2 hours. After filtration, methanol was evaporated under a reduced pressure and the residue was made basic with an addition of 4N sodium hydroxide. The iron oxide precipitated was separated by filtration, washed with methylene chloride (50 ml). Also the filtrate was extracted with methylene (50 ml×2) and combined with the methylene chloride washing, followed by drying over anhydrous sodium sulfate. Evaporation of the solvent gave N,N-diethyl-3-(amino)benzenesulfonamide (3.0 g) (m.p. 82°-84° C.).

후처리

  1. additionwas added
  2. filtrationAfter filtration, methanol
  3. customwas evaporated under a reduced pressure
  4. additionthe residue was made basic with an addition of 4N sodium hydroxide
  5. customThe iron oxide precipitated
  6. customwas separated by filtration
  7. washwashed with methylene chloride (50 ml)
  8. extractionAlso the filtrate was extracted with methylene (50 ml×2)
  9. dry with materialby drying over anhydrous sodium sulfate
  10. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-5f51a9bab7004a12956b43190044f6f3
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04976773

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