Stannous Chloride → 3-amino-N,N-dimethylbenzene-1-sulfonamide

HRID 1814646

反応式

HRID 1814646 の反応式
[CH3:1][N:2]([CH3:15])[S:3]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N+:12]([O-])=O)[CH:7]=1)(=[O:5])=[O:4].Cl[Sn]Cl>C(O)C>[NH2:12][C:8]1[CH:7]=[C:6]([S:3]([N:2]([CH3:15])[CH3:1])(=[O:5])=[O:4])[CH:11]=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 24479Stannous ChlorideHCID 224495N,N-Dimethyl 3-nitrobenzenesulfonamide

生成物 1

HCID 2355203-amino-N,N-dimethylbenzene-1-sulfonamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of the above N,N-dimethyl-3-nitro-benzenesulfonamide (20.4 mmol, 4.7 g) in ethanol (50 mL) was added SnCl2 (105 mmol, 19.9 g) and the mixture was refluxed for 1 hour. Upon cooling, the solvent was removed in vacuo. Ethyl acetate (200 mL) and NaHCO3 (sat, 100 mL) were added to the residue followed by another 200 mL ethyl acetate and 500 mL water. The phases were separated and the organic phase was washed twice with water. The organic phase was filtered, washed with water (2×100 mL) dried over MgSO4 and evaporated to leave the title compound.

後処理

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperatureUpon cooling
  3. customthe solvent was removed in vacuo
  4. additionEthyl acetate (200 mL) and NaHCO3 (sat, 100 mL) were added to the residue
  5. customThe phases were separated
  6. washthe organic phase was washed twice with water
  7. filtrationThe organic phase was filtered
  8. washwashed with water (2×100 mL)
  9. dry with materialdried over MgSO4
  10. customevaporated

出典と根拠

ORDレコード
ord-4651545c77b84eecad76b81525b363f8
出典データセット
uspto-grants-2005_04
特許番号
US06875760B2

関連ノート

読み込み中…