HCID 23114063, compound → HCID 23114294, compound

HRID 1787150Notes

Reaction equation

HRID 1787150 reaction equation
C(C1C=CC=C(OC)C=1C(=O)COC1C=C(C)C=C(C)C=1C)(C)C.[CH:25]([C:28]1[CH:33]=[CH:32][C:31]([C:34](=O)[CH2:35][O:36][C:37]2[CH:42]=[C:41]([CH3:43])[CH:40]=[C:39]([CH3:44])[C:38]=2[CH3:45])=[C:30]([O:47][CH3:48])[CH:29]=1)([CH3:27])[CH3:26].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:25]([C:28]1[CH:33]=[CH:32][C:31]([C:34]2[C:42]3[C:41]([CH3:43])=[CH:40][C:39]([CH3:44])=[C:38]([CH3:45])[C:37]=3[O:36][CH:35]=2)=[C:30]([O:47][CH3:48])[CH:29]=1)([CH3:27])[CH3:26]

Participants

5

Reactant 3

HCID 23114063HCID 23114063, compoundHCID 23114381HCID 23114381, compoundHCID 71586775Bentonite

Product 1

HCID 23114294HCID 23114294, compoundYield 40%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
90 °C

Procedure

A mixed solution of the mixture of 1-(2-isopropyl-6-methoxyphenyl)-2-(2,3,5-trimethylphenoxy)ethanone and 1-(4-isopropyl-2-methoxyphenyl)-2-(2,3,5-trimethylphenoxy)ethanone obtained in Reference Example 171 (6.27 g, 19.2 mmol) and Montmorillonite KSF (9.40 g) in toluene (100 mL) was stirred under argon atmosphere at 90° C. for 5 hours. The reaction solution was filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate hexane=15:85) to obtain 2.34 g (yield 40%) of the title compound. Oily matter.

Workup

  1. filtrationThe reaction solution was filtered through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by silica gel chromatography (ethyl acetate hexane=15:85)

Sources & evidence

ORD record
ord-bfe74ebc06ad485890352a030f64f82c
Source dataset
uspto-grants-2009_03
Patent number
US07507841B2

Reaction notes

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