Sulfuric Acid → 891657-51-5

HRID 547277ノート

反応式

HRID 547277 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 22615934891657-51-5

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
4 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6a71d20463354bff8c3df10618465825
出典データセット
uspto-grants-2011_05
特許番号
US07939521B2

反応ノート

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