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

HRID 1110673ノート

反応式

HRID 1110673 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 29635153-Amino-N,N-diethylbenzene-1-sulfonamide収率 87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-5f51a9bab7004a12956b43190044f6f3
出典データセット
uspto-grants-1990_12
特許番号
US04976773

反応ノート

読み込み中…