Acrylonitrile → 3-(4-Methoxyphenoxy)propanenitrile

HRID 610388

反応式

HRID 610388 の反応式
[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]

参加物

6

反応物 3

HCID 7855AcrylonitrileHCID 90154-MethoxyphenolHCID 14797Potassium Hydroxide

生成物 1

HCID 1142473-(4-Methoxyphenoxy)propanenitrile

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6386tert-Butanol溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-ebb828bdced2423db50b0cb15ce2fc20
出典データセット
uspto-grants-1999_12
特許番号
US05998451

関連ノート

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