Acetic Acid → HCID 13347277、化合物

HRID 1098762ノート

反応式

HRID 1098762 の反応式
[C:1]([C:4]1[CH:11]=[CH:10]C(C#N)=[C:6]([Br:12])[CH:5]=1)(=[O:3])[CH3:2].[OH-].[Na+].[CH3:15][C:16]([OH:18])=[O:17]>O.OS(O)(=O)=O>[C:1]([C:4]1[CH:11]=[CH:10][C:15]([C:16]([OH:18])=[O:17])=[C:6]([Br:12])[CH:5]=1)(=[O:3])[CH3:2]

参加物

6

反応物 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 133472764-Acetyl-2-bromobenzonitrile

生成物 1

HCID 13347277HCID 13347277、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

実験手順

A solution of the product obtained in step 2 (0.5 g, 2.23 mmol) in AcOH (2.5 mL), H2O (2.5 mL) and concentrated H2SO4 (2.5 mL) was refluxed for 5 h. After cooling, the reaction mixture was adjusted with 10 N NaOH to pH=10 and washed with AcOEt. The aqueous layer was acidified with concentrated HCl to pH=1 and then extracted with AcOEt. The organic phase was washed with H2O, dried over Na2SO4 and evaporated under reduced pressure. The crude product was used in the following step without further purification.

後処理

  1. temperatureAfter cooling
  2. washwashed with AcOEt
  3. extractionextracted with AcOEt
  4. washThe organic phase was washed with H2O
  5. dry with materialdried over Na2SO4
  6. customevaporated under reduced pressure
  7. customThe crude product was used in the following step without further purification

出典と根拠

ORDレコード
ord-c1267523512b47bb811029123f96d168
出典データセット
uspto-grants-2012_03
特許番号
US08143242B2

反応ノート

読み込み中…