Acrylonitrile → 3-(4-Methoxyphenoxy)propanenitrile

HRID 610388

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HRID 610388 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[OH-].[K+].[C:12](#[N:15])[CH:13]=[CH2:14]>C(O)(C)(C)C.CCOCC>[C:12]([CH2:13][CH2:14][O:9][C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)#[N:15]

참가 물질

6

반응물 3

HCID 7855AcrylonitrileHCID 90154-MethoxyphenolHCID 14797Potassium Hydroxide

생성물 1

HCID 1142473-(4-Methoxyphenoxy)propanenitrile

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6386tert-Butanol용매

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온도
75 °C

실험 절차

4-Methoxyphenol (248 g), KOH (5.6 g) and acrylo-nitrile (397 ml) were dissolved in 1 liter of t-butanol and heated with stirring at 75° C. for 5 hours. The mixture was then cooled to room temperature and stripped in vacuo to solid residue, which was repulped in ether and insolubles recovered by filtration. The latter were taken up in 2 liters of ethyl acetate, washed in sequence with 1 liter each of H2O, saturated NaHCO3 and saturated NaCl, dried over MgSo4 and restripped to yield purified title product, 199.4 g, m.p. 62-64° C.

후처리

  1. temperatureheated
  2. temperatureThe mixture was then cooled to room temperature
  3. filtrationinsolubles recovered by filtration
  4. washwashed in sequence with 1 liter each of H2O, saturated NaHCO3 and saturated NaCl
  5. customdried over MgSo4
  6. customto yield
  7. custompurified title product, 199.4 g, m.p. 62-64° C.

출처 및 근거

ORD 기록
ord-ebb828bdced2423db50b0cb15ce2fc20
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998451

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