Water → 2-Bromo-1,3-dimethyl-4-nitrobenzene

HRID 1182265

反応式

HRID 1182265 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[CH:6][C:5]=1[CH3:11])([O-:3])=[O:2].S(=O)(=O)(O)O.O.[Br:18]([O-])(=O)=O.[K+]>C(O)(=O)C>[Br:18][C:6]1[C:5]([CH3:11])=[C:4]([N+:1]([O-:3])=[O:2])[CH:9]=[CH:8][C:7]=1[CH3:10]

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 69914-Nitro-m-xyleneHCID 23673461Potassium Bromate

生成物 1

HCID 123959052-Bromo-1,3-dimethyl-4-nitrobenzene

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 4-nitro-m-xylene (0.96 g, 6.4 mmol) in acetic acid (8 mL) and sulfuric acid (4 g) and Water (4 mL) was added potassium bromate (1.18 g, 7 mmol) portion-wise over 20 minutes. The mixture was allowed to stir 72 hours at room temperature. The desired product was recovered together with starting material after partition between water, and ethyl acetate (2×) washing with water, saturated sodium bicarbonate solution and brine. The organic layer was dried over sodium sulfate, decanted and upon concentration under reduced pressure yielded the desired 2-bromo-1,3-dimethyl-4-nitrobenzene and starting material as an oily solid. The crude mixture was carried on to step two without further purification.

後処理

  1. customThe desired product was recovered together with starting material
  2. customafter partition between water, and ethyl acetate (2×)
  3. washwashing with water, saturated sodium bicarbonate solution and brine
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customdecanted and upon concentration under reduced pressure

出典と根拠

ORDレコード
ord-0ebfab3781c344288918b13406048e65
出典データセット
uspto-grants-2007_10
特許番号
US07288538B2

関連ノート

読み込み中…