phenyl 4-chlorobenzoate synthesis
- Product Name:phenyl 4-chlorobenzoate
- CAS Number:1871-38-1
- Molecular formula:C13H9ClO2
- Molecular Weight:232.66
Yield:1871-38-1 97.1%
Reaction Conditions:
with 1,4-diaza-bicyclo[2.2.2]octane;1,1'-bis-(diphenylphosphino)ferrocene;tris-(dibenzylideneacetone)dipalladium(0);1-ethyl-3-methylimidazolium tetrafluoroborate in N,N-dimethyl-formamide at 20 - 90; for 10 h;Reagent/catalyst;
Steps:
2 Example 2
At room temperature to an appropriate amount of DMF, 100mmol compounds of formula (I), 250mmol compound of the formula (II), 15mmol composite catalyst (Pd2 (dba) 3 and DPPF mixture of both the molar ratio of 1: 0.2), 25mmol 1 - ethyl-3-methylimidazolium tetrafluoroborate and 250mmol DABCO, then warmed to 90 , and the reaction was stirred at this temperature for 10 hours. After completion of the reaction, the reaction system was cooled to room temperature, then added mass% concentration of a 10% aqueous hydrochloric acid, adjusting the pH value of 6.5-7; ethyl acetate with a sufficient amount of 2-4 times, the combined organic phases, with no over anhydrous sodium sulfate, concentrated in vacuo, the residue was purified by column chromatography over silica gel 200-300 mesh, a mixed solvent of acetone and petroleum ether as eluent, wherein the volume ratio of acetone to petroleum ether is 1: 3, to give the compounds of formula (III), a yield of 97.1%
References:
CN104876820,2016,B Location in patent:Paragraph 0041; 0042; 0043; 0044; 0045; 0046
