Hydrochloric Acid → Methyl 5-cyano-2-methylbenzoate

HRID 232869

反応式

HRID 232869 の反応式
Br[C:2]1[CH:3]=[C:4]([C:9]([O:11][CH3:12])=[O:10])[C:5]([CH3:8])=[CH:6][CH:7]=1.O.Cl.[CH3:15][N:16](C)C=O>>[C:15]([C:2]1[CH:3]=[C:4]([C:9]([O:11][CH3:12])=[O:10])[C:5]([CH3:8])=[CH:6][CH:7]=1)#[N:16]

参加物

5

実験手順

0.5 g of cuprous cyanide was added to 1 g of methyl 4-bromo-o-toluate obtained in Reference example 18 dissolved in 0.7 ml of dimethylformamide and the mixture was refluxed under heating for 6 hours. Then, to the reaction mixture were added 2.6 ml of water, 0.5 ml of conc. hydrochloric acid and 1.75 g of ferric chloride and the mixture was stirred at 60° to 70° C. for 30 minutes. After the reaction mixture was extracted with ethyl acetate, the organic layer was washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed from the solution to obtain 0.76 g of the title compound.

後処理

  1. customobtained in Reference example 18
  2. temperaturethe mixture was refluxed
  3. temperatureunder heating for 6 hours
  4. extractionAfter the reaction mixture was extracted with ethyl acetate
  5. washthe organic layer was washed with a saturated saline solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was removed from the solution

出典と根拠

ORDレコード
ord-0a46ed268c724a50bce1ceb17529e8a6
出典データセット
uspto-grants-1997_01
特許番号
US05591752

関連ノート

読み込み中…