Water → 2-Nitrophenylacetonitrile

HRID 1462323

反応式

HRID 1462323 の反応式
O.[N+:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11][C:12](=[N:16]O)C(O)=O)([O-:4])=[O:3]>C(O)(=O)C>[N+:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11][C:12]#[N:16])([O-:4])=[O:3]

参加物

4

反応物 2

HCID 962WaterHCID 714366072-(Hydroxyimino)-3-(2-nitrophenyl)propanoic acid

生成物 1

HCID 118882-Nitrophenylacetonitrile

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Water (50,000 ml), 2,940 ml of glacial acetic acid and (22.22 moles) of 2-nitrophenylpyruvic acid oxime were charged into a 20 gallon reactor. The stirred suspension was heated over two hours under nitrogen atmosphere to 90° and this temperature was maintained for 2 hours. The dark solution was allowed to cool slowly and was stirred overnight at ambient temperature. The suspension was extracted with 5×4,000 ml of methylene chloride, washed with 3×3,000 ml of water, dried over magnesium sulfate and filtered. The filtrate was treated with activated carbon, filtered and the solvent was removed under reduced pressure. The solid residue was recrystallized from 1,000 ml of isopropanol to give 2-nitrophenylacetonitrile, m.p. 82°-84°.

後処理

  1. temperatureThe stirred suspension was heated over two hours under nitrogen atmosphere to 90°
  2. temperaturethis temperature was maintained for 2 hours
  3. temperatureto cool slowly
  4. extractionThe suspension was extracted with 5×4,000 ml of methylene chloride
  5. washwashed with 3×3,000 ml of water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. additionThe filtrate was treated with activated carbon
  9. filtrationfiltered
  10. customthe solvent was removed under reduced pressure
  11. customThe solid residue was recrystallized from 1,000 ml of isopropanol

出典と根拠

ORDレコード
ord-5578a2c75bf84cf884b9a34b11c22857
出典データセット
uspto-grants-1984_07
特許番号
US04460508

関連ノート

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