Hydrochloric Acid → 2-Chloro-4-hydroxybenzaldehyde

HRID 62890

反応式

HRID 62890 の反応式
[Cl:1][C:2]1[CH:9]=[C:8]([OH:10])[CH:7]=[CH:6][C:3]=1[C:4]#N.CC(C[AlH]CC(C)C)C.Cl.C1C[O:24]CC1>>[Cl:1][C:2]1[CH:9]=[C:8]([OH:10])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:24]

参加物

5

反応条件

温度
-78 °C

実験手順

After 2-chloro-4-hydroxy-benzonitrile (2 g, 0.013 mol) was dissolved in anhydrous THF (40 mL), DIBAL-H 1M hexane solution (21.7 mL, 0.032 mol) was added thereto at −78° C., and the mixture was stirred for 1 hour, and then stirred at room temperature for 2 hours. After the termination of the reaction, the reactant was added with 1M HCl at 0° C. and then extracted with EtOAc. The organic layer was separated, dried with MgSO4, and concentrated under reduced pressure to obtain the title compound, which was used in the next step without a separate purification process.

後処理

  1. stirringstirred at room temperature for 2 hours
  2. customAfter the termination of the reaction
  3. extractionextracted with EtOAc
  4. customThe organic layer was separated
  5. dry with materialdried with MgSO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-40264fe6f229486c8612a904a343b595
出典データセット
uspto-grants-2016_09
特許番号
US09447044B2

関連ノート

読み込み中…