(3-NITROPHENYL)-PROPYNOIC ACID synthesis
- Product Name:(3-NITROPHENYL)-PROPYNOIC ACID
- CAS Number:4996-15-0
- Molecular formula:C9H5NO4
- Molecular Weight:191.14
124-38-9
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4996-15-0
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Yield:4996-15-0 95%
Reaction Conditions:
with caesium carbonate in dimethyl sulfoxide at 60; for 24 h;Sealed tube;Inert atmosphere;
Steps:
34 Example 34: Reaction of 3-nitrophenylacetylene and carbon dioxide involved in cesium carbonate at 60 ° C:
Under sealed conditions without water and oxygen, argon protection,0.6516 g of Cs2CO3 (2 mmol, 2 equiv.) was weighed into the reaction flask.A micro syringe was charged with 0.1471 g (1 mmol, 1 equiv.) 3-nitrophenylacetylene.Add 5 mL of DMSO to the syringe.The air in the reaction system was replaced by CO 2 gas, and reacted at 60 ° C for 24 hours.After the reaction, the mixture was exposed to air, cooled slightly at room temperature, and then cooled in an ice water bath.Add 10 mL of deionized water, and add 20 mL of 6 mol/L HCl solution to fully acidify.The organic phase was combined and the organic phase was washed with brine brine.The organic phase is separated and dried with anhydrous Na2SO4.The solvent is removed under reduced pressure to obtain the desired product.The isolated yield was 95%.
References:
CN108558635,2018,A Location in patent:Paragraph 0139; 0140; 0141
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