Aluminum(III) Chloride → HCID 19016867, compound

HRID 1728972Notes

Reaction equation

HRID 1728972 reaction equation
[CH3:1][C:2]1[CH:14]=[CH:13][CH:12]=[CH:11][C:3]=1[CH2:4][CH:5]([CH2:9][CH3:10])[C:6](Cl)=[O:7].[Al+3].[Cl-].[Cl-].[Cl-]>C1(C)C=CC=CC=1>[CH2:9]([CH:5]1[CH2:4][C:3]2[C:11](=[CH:12][CH:13]=[CH:14][C:2]=2[CH3:1])[C:6]1=[O:7])[CH3:10]

Participants

4

Reactant 2

HCID 6451240Aluminum(III) ChlorideHCID 19016864HCID 19016864, compound

Product 1

HCID 19016867HCID 19016867, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
80 °C

Procedure

101.7 g (0.48 mol) of 2-(2-methyl-benzyl)-butyryl chloride (e2) were added dropwise to 191 g (1.43 mol) of AlCl3 in 600 ml of toluene, and the mixture was heated at 80° C. for about 3.5 hours. The reaction mixture was poured onto 1 l of ice/concentrated HCl, and the phases were separated. The aqueous phase was extracted 4 times with 250 ml of toluene each time, and the combined organic phases were washed with saturated aqueous NaHCO3 solution and NaCl solution and dried over MgSO4. The solvent was removed in vacuo and the residue was distilled (78° C./0.2 mmHg).

Workup

  1. customthe phases were separated
  2. extractionThe aqueous phase was extracted 4 times with 250 ml of toluene each time
  3. washthe combined organic phases were washed with saturated aqueous NaHCO3 solution and NaCl solution
  4. dry with materialdried over MgSO4
  5. customThe solvent was removed in vacuo
  6. distillationthe residue was distilled (78° C./0.2 mmHg)

Sources & evidence

ORD record
ord-62485f68e7e2466fb607327cdf1461e7
Source dataset
uspto-grants-1994_07
Patent number
US05329033

Reaction notes

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