Water → 2-Nitrophenylacetonitrile

HRID 1462168

반응식

HRID 1462168 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 118882-Nitrophenylacetonitrile

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-9c09d08e3a6843a695830f8b8492816a
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04459232

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