Benzene → HCID 12659614, compound

HRID 1377430Notes

Reaction equation

HRID 1377430 reaction equation
[CH3:1]I.[CH:3]1[CH:8]=[CH:7][CH:6]=[CH:5]C=1.C([O:11][CH2:12][CH3:13])C>>[CH2:8]([CH:7]([CH2:6][CH3:5])[CH2:1][C:12](=[O:11])[CH3:13])[CH3:3]

Participants

4

Reactant 3

HCID 241BenzeneHCID 3283Diethyl EtherHCID 6328Methyl iodide

Product 1

HCID 12659614HCID 12659614, compound

Procedure

85.2 g methyl iodide in 50 ml of diethyl ether are added dropwise. Thereafter, 100 ml of benzene are added, and a part of the diethylether is distilled off. After addition of 33.3 g of ethyl-2-butyl-carbonitrile 19b, the mixture is heated under reflux for 5 hours. The reaction mixture is hydrolyzed with NH4Cl-solution, extracted with diethyl ether, washed with water, dried over sodium sulfate, concentrated, and distilled in vacuo over a Vigreux column. Obtained are:

Workup

  1. distillationa part of the diethylether is distilled off
  2. additionAfter addition of 33.3 g of ethyl-2-butyl-carbonitrile 19b
  3. temperaturethe mixture is heated
  4. temperatureunder reflux for 5 hours
  5. extractionextracted with diethyl ether
  6. washwashed with water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated
  9. distillationdistilled in vacuo over a Vigreux column
  10. customObtained

Sources & evidence

ORD record
ord-da4f63a1ce284807bda5b224fcd682e4
Source dataset
uspto-grants-1997_09
Patent number
US05665716

Reaction notes

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