HCID 23114241, compound → HCID 23114293, compound

HRID 2376314Notes

Reaction equation

HRID 2376314 reaction equation
[CH:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=O)[CH2:11][O:12][C:13]2[CH:18]=[C:17]([CH3:19])[CH:16]=[C:15]([CH3:20])[CH:14]=2)=[CH:6][CH:5]=1)([CH3:3])[CH3:2].O.[O-2].[O-2].[O-2].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.[Al+3].[Al+3]>C1(C)C=CC=CC=1>[CH:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:14]3[C:15]([CH3:20])=[CH:16][C:17]([CH3:19])=[CH:18][C:13]=3[O:12][CH:11]=2)=[CH:6][CH:5]=1)([CH3:3])[CH3:2]

Participants

4

Reactant 2

HCID 23114241HCID 23114241, compoundHCID 71586775Bentonite

Product 1

HCID 23114293HCID 23114293, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
95 °C

Procedure

A solution of 1-(4-isopropylphenyl)-2-(3,5-dimethylphenoxy)ethanone obtained in Reference Example 142 (38.1 g, 135 mmol) and Montmorillonite KSF (57.2 g) in toluene (400 mL) was heated at 95° C., and was reacted for 16 hours. The reaction solution was cooled to room temperature, and then Montmorillonite KSF was filtered off. The solution was purified by silica gel column chromatography (ethyl acetate:hexane=1:9), and the solvent was distilled off under reduced pressure to obtain 35.6 g (yield 100%) of the title compound as an oily matter. The oily matter was, if necessary, crystallized with methanol. Melting point: 44-45° C.

Workup

  1. customwas reacted for 16 hours
  2. temperatureThe reaction solution was cooled to room temperature
  3. filtrationMontmorillonite KSF was filtered off
  4. customThe solution was purified by silica gel column chromatography (ethyl acetate:hexane=1:9)
  5. distillationthe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-7ca406a577f14ffd822c481e3539856b
Source dataset
uspto-grants-2008_12
Patent number
US07465815B2

Reaction notes

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