Ammonium Hydroxide → 2-Tert-butyl-5-nitrobenzene-1-sulfonamide

HRID 423903ノート

反応式

HRID 423903 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:6]=1[S:14](Cl)(=[O:16])=[O:15])([CH3:4])([CH3:3])[CH3:2].[NH4+:18].[OH-]>CCOCC.O>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:6]=1[S:14]([NH2:18])(=[O:16])=[O:15])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 2

HCID 14923Ammonium HydroxideHCID 574702642-Tert-butyl-5-nitrobenzene-1-sulfonyl chloride

生成物 1

HCID 574702652-Tert-butyl-5-nitrobenzene-1-sulfonamide収率 34%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 2-tert-butyl-5-nitrobenzene-1-sulfonyl chloride (100 mg, 0.36 mmol) in ether (2 mL) was added aqueous NH4OH (128 μL, 3.6 mmol) at 0° C. The mixture was stirred at room temperature overnight, diluted with water and extracted with ether. The combined ether extracts were washed with brine and dried over Na2SO4. After removal of solvent, the residue was purified by column chromatography (0-50% EtOAc-Hexane) to give 2-tert-butyl-5-nitrobenzene-1-sulfonamide (31.6 mg, 34%).

後処理

  1. extractionextracted with ether
  2. washThe combined ether extracts were washed with brine
  3. dry with materialdried over Na2SO4
  4. customAfter removal of solvent
  5. customthe residue was purified by column chromatography (0-50% EtOAc-Hexane)

出典と根拠

ORDレコード
ord-7032f10aa9c34349887e2f9e981e1b59
出典データセット
uspto-grants-2012_01
特許番号
US08101767B2

反応ノート

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