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[ CAS No. 63506-58-1 ] {[proInfo.proName]}

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Chemical Structure| 63506-58-1
Chemical Structure| 63506-58-1
Structure of 63506-58-1 * Storage: {[proInfo.prStorage]}
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Product Details of [ 63506-58-1 ]

CAS No. :63506-58-1 MDL No. :MFCD06204198
Formula : C15H14O3 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 242.27 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 63506-58-1 ]

* 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 [ 63506-58-1 ]

[ 63506-58-1 ] Synthesis Path-Downstream   1~3

  • 2
  • [ 529-28-2 ]
  • [ 610-94-6 ]
  • [ 93-58-3 ]
  • [ 4877-93-4 ]
  • [ 792-74-5 ]
  • [ 63506-58-1 ]
  • 3
  • [ 610-94-6 ]
  • [ 5720-06-9 ]
  • [ 63506-58-1 ]
YieldReaction ConditionsOperation in experiment
99% With palladium diacetate; sodium carbonate; triphenylphosphine In water; toluene for 3.5h; Heating;
92% With tetrakis(triphenylphosphine) palladium(0); tetrabutylammomium bromide; potassium carbonate In ethanol; water; toluene at 78 - 80℃; for 8h; Inert atmosphere; 1.1 (1) intermediate 1(compound 1)synthesis of intermediate 2(compound 2) In a 1 L three-necked flask equipped with a thermometer and a condenser, 30 g of o-methoxybenzonic acid, 43 g of methyl o-bromobenzoate, 55 g of k2CO3, and 13 g of TBABA were sequentially added, and then 300 ml of toluene, 100 ml of ethanol, and 50 ml of water were added in this order, and replaced with nitrogen. Add 1.15g of Pd(PPH3)4 to the air in the reaction bottle under nitrogen protection, turn on the heating, magnetically stir, and heat to (78 80 ) to reflux the reaction. After 8 hours of reaction, take a sample and test, and stop the reaction when the raw material reaction is complete. After cooling down to room temperature for post-treatment, the reaction solution was filtered, left to separate, and the aqueous layer was extracted with 100 ml of toluene. The organic phases were combined, washed with water to neutrality, dried over anhydrous Na2SO4 for 1 h, and filtered to remove the drying agent to obtain a filter cake. The filter cake was rinsed with a small amount of toluene, and the filtrates were combined. The filtrates were concentrated and purified by column to obtain the target product Intermediate 2. Intermediate 2 is a colorless liquid 44g, yield 92%,
With dichloro[1,1'-bis(di-t-butylphosphino)ferrocene]palladium(II); potassium carbonate In water; acetonitrile at 60℃; Inert atmosphere; Sealed vessel; 4.6. Typical preparative procedure Typical preparative procedures were performed on 10.0 mmol scale using a Mettler-Toledo FlexiWeigh 30 automated solid handling unit to pre-weigh the aryl halide (10.0 mmol, 1.0 equiv), aryl boronic acid (12.0 mmol, 1.2 equiv) and Pd-118 (65.2 mg, 0.1 mmol, 1.0 mol %). Acetonitrile (10.0 mL) was added, followed by K2CO3 added as a stock aqueous solution (10.0 mL water containing 2.07 g, 15.0 mmol, 1.5 equiv). NB. No internal standard was added for preparative reactions. Reaction mixtures were sealed under a N2 atmosphere and heated to 60 °C with magnetic stirring. HPLC analysis showed that reactions using aryl bromides were complete within 1 h but that aryl chlorides typically required 24 h.After reaction mixtures had cooled to room temperature, stirring was stopped and the phases were allowed to separate. The lower aqueous phase was removed and discarded (cutting away any interfacial catalyst residues if present) and the acetonitrile phase concentrated to dryness to give typically a light to dark brown solid or dark-coloured gum. Solids were triturated with methanol (20 mL) for 1-2 h, then isolated by filtration, washed once or twice with methanol (4 mL each wash) and dried under vacuum. Oils were purified by flash silica gel chromatography as noted below. All isolated compounds gave 1H NMR data in agreement with published values. Literature data is given for mp values for comparison.
With 1,1'-bis-(diphenylphosphino)ferrocene; potassium phosphate; palladium diacetate In 1,2-dimethoxyethane at 80℃; for 12h; Inert atmosphere; Schlenk technique;

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