Sulfuric Acid → 891657-51-5

HRID 547277노트

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HRID 547277 반응식
N[C:2]1[CH:3]=[C:4]([CH:8]([CH3:11])[C:9]#[N:10])[CH:5]=[CH:6][CH:7]=1.[OH:12]S(O)(=O)=O.N([O-])=O.[Na+].C(OCC)(=O)C>O>[OH:12][C:2]1[CH:3]=[C:4]([CH:8]([CH3:11])[C:9]#[N:10])[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 8857Ethyl AcetateHCID 134713392-(3-Aminophenyl)propanenitrileHCID 23668193Sodium Nitrite

생성물 1

HCID 22615934891657-51-5

시약·촉매·용매 1

HCID 962Water용매2회

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온도
4 °C

실험 절차

2-(3-aminophenyl)propionitrile (1.0 g, 6.75 mmol), was suspended in water (12 mL), then under vigorous stirring, H2SO4 (1.5 ml, 27 mmol) was added dropwise. After stirring 20 min, the mixture was cooled to 4° C., a solution of NaNO2 (0.466 g, 6.75 mmol) in water (5 mL) was added dropwise and the resulting solution was left stirring at reflux 1 h. After cooling at room temperature, ethyl acetate (10 mL) was added to the mixture, the crude was extracted and the organic phase washed with water (3×10 mL) and brine (3×10 mL). After drying over Na2SO4 and solvent evaporation under reduced pressure 2-(3-hydroxyphenyl)propionitrile was obtained as yellow oil in nearly quantitative yield.

후처리

  1. waitthe resulting solution was left
  2. stirringstirring
  3. temperatureat reflux 1 h
  4. temperatureAfter cooling at room temperature
  5. extractionthe crude was extracted
  6. washthe organic phase washed with water (3×10 mL) and brine (3×10 mL)
  7. dry with materialAfter drying over Na2SO4 and solvent evaporation under reduced pressure 2-(3-hydroxyphenyl)propionitrile
  8. customwas obtained as yellow oil in nearly quantitative yield

출처 및 근거

ORD 기록
ord-6a71d20463354bff8c3df10618465825
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939521B2

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