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Chemical Structure| 631-25-4 Chemical Structure| 631-25-4

Structure of 631-25-4

Chemical Structure| 631-25-4

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Product Details of [ 631-25-4 ]

CAS No. :631-25-4
Formula : C27H26O7
M.W : 462.49
SMILES Code : O=C(CC(C(OCC1=CC=CC=C1)=O)(O)CC(OCC2=CC=CC=C2)=O)OCC3=CC=CC=C3

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Application In Synthesis of [ 631-25-4 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 631-25-4 ]

[ 631-25-4 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 100-39-0 ]
  • [ 68-04-2 ]
  • [ 631-25-4 ]
YieldReaction ConditionsOperation in experiment
85% In a 2 L separable flask equipped with a cooling tube, 46.6 g (0.14 mol) of <strong>[68-04-2]sodium citrate</strong> dihydrate,14.4 g (0.04 mol) of tetrabutylammonium bromide,285 g (3.9 mol) of N, N-dimethylformamide were charged,The mixture was heated up to 80 C. with stirring with an oil bath.147.9 g (0.86 mol) of benzyl bromide was added dropwise over 30 minutes,After heating and stirring for 7.5 hours, 20.9 g (0.21 mol) of triethylamine,Was slowly added dropwise over 2 hours,After completion, the mixture was stirred for about 10 minutes.After cooling, the mixture was distilled under reduced pressure. To the concentrate obtained, 320 mL of ethyl acetate,430 mL of pure water was added.After insoluble matter was removed by vacuum filtration,The aqueous layer was separated,Further, 200 mL of saturated sodium chloride aqueous solution was added,After washing the oil layer,The aqueous layer was separated.The oil layer was distilled off under reduced pressure, and 110 mL of ethanol was added to the residue,Heated to 65 C,After dissolving the residue,A solid precipitated by cooling. After filtration under reduced pressure,40 CTo give 56.6 g (yield 85%) of tribenzyl citrate as a white solid.
  • 2
  • [ 68-04-2 ]
  • [ 100-51-6 ]
  • [ 631-25-4 ]
YieldReaction ConditionsOperation in experiment
88% With toluene-4-sulfonic acid; In toluene;Inert atmosphere; Reflux; Reference Example 2:A 2 L eggplant flask equipped with a Dean-Stark apparatus was charged with <strong>[68-04-2]sodium citrate</strong> dihydrate19.5 g (0.07 mol),45.9 g (0.24 mol) of toluenesulfonic acid monohydrate,100 g (0.92 mol) of benzyl alcohol,200 mL of toluene was charged,Under a nitrogen atmosphere,And the mixture was stirred under reflux.After cooling down,500 mL of ethyl acetate was added,And stirred well.This was stirred little by little into a 5 L beaker containing 1 L of a 5% by mass sodium bicarbonate aqueous solutionWhile stirring.Excluding insoluble matter,After separating the aqueous layer,The organic layer was washed with water,And then dried over anhydrous sodium sulfate.When the solvent and benzyl alcohol were distilled off under reduced pressure and the residue obtained was analyzed by LC method,The yield of tribenzyl citrate in the ingredients was 27.0 g (88% yield).
 

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