Sulfuric Acid → 6-Chloro-2-hydroxy-3-nitrobenzenesulfonamide

HRID 2301492ノート

反応式

HRID 2301492 の反応式
C([C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([Cl:13])[C:5]=1[S:14]([NH2:17])(=[O:16])=[O:15])(=O)C.Cl[Si](C)(C)C.S(=O)(=O)(O)[OH:24]>CO>[Cl:13][C:6]1[C:5]([S:14]([NH2:17])(=[O:16])=[O:15])=[C:4]([OH:24])[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 6397ChlorotrimethylsilaneHCID 183734452-Acetyl-6-chloro-3-nitrobenzenesulfonamide

生成物 1

HCID 112768176-Chloro-2-hydroxy-3-nitrobenzenesulfonamide収率 68%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2-acetyl6-chloro-3-nitrobenzenesulfonamide (1.72 g, 5.83 mmol), chlorotrimethylsilane (2 mL) and fuming sulfuric acid (0.5 mL) in methanol was heated to reflux for 20 hours. The solvent was evaporated. The residue was diluted with ethyl acetate and washed with water. The organic layer was then dried (Na2SO4) and concentrated to give the desired product (1.0 g, 68%). EI-MS (m/z) 251.1, 253.2 (M−).

後処理

  1. temperatureto reflux for 20 hours
  2. customThe solvent was evaporated
  3. additionThe residue was diluted with ethyl acetate
  4. washwashed with water
  5. dry with materialThe organic layer was then dried (Na2SO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-876eafb779e441418151c09417b56faa
出典データセット
uspto-grants-2002_12
特許番号
US06500863B1

反応ノート

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