Sulfuric Acid → 3-(2-Chloro-phenyl)-3-oxo-propionamide

HRID 1667659

反応式

HRID 1667659 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:12])[CH2:9][C:10]#[N:11].S(=O)(=O)(O)[OH:14]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:12])[CH2:9][C:10]([NH2:11])=[O:14]

参加物

3

反応物 2

HCID 1118Sulfuric AcidHCID 27342012-Chlorobenzoylacetonitrile

生成物 1

HCID 866427963-(2-Chloro-phenyl)-3-oxo-propionamide

実験手順

A mixture of 17.0 g (94.65 mmole) of 3-(2-chloro-phenyl)-3-oxo-propionitrile and 50 mL of sulfuric acid was stirred at room temperature for 18 hours. The mixture was poured into ice-water and extracted three times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium carbonate solution and brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography eluting with ethyl acetate-hexanes (gradient 20:80-70:30) to give 14.12 g of 3-(2-chloro-phenyl)-3-oxo-propionamide.

後処理

  1. extractionextracted three times with ethyl acetate
  2. washThe combined organic phases were washed with saturated aqueous sodium carbonate solution and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography
  7. washeluting with ethyl acetate-hexanes (gradient 20:80-70:30)

出典と根拠

ORDレコード
ord-1c03274c4acb49079d28150685097457
出典データセット
uspto-grants-2011_10
特許番号
US08044213B2

関連ノート

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