Acetylsalicylic acid synthesis
- Product Name:Acetylsalicylic acid
- CAS Number:50-78-2
- Molecular formula:C9H8O4
- Molecular Weight:180.16
Yield:50-78-2 100%
Reaction Conditions:
in neat (no solvent);Molecular sieve;Microwave irradiation;Green chemistry;
Steps:
Optimized MW-assisted peracetylation
General procedure: The substrate belonging to one of the subset reported in Table 1(NTC, TC, CP, DGNP) (0.1 mmol) was left to react under MWheating (Synthos 3000, Anton Paar) with dry acetic anhydride(1 mL, 10 mmol) in a 3 mL vial (Rotor 64MG5 ), equipped witha magnetic stirrer in the presence of molecular sieves(10 % w/w). The microwave, equipped with IR sensor forexternal temperature control (IR limit calculated as follows:Tinternal= 1.214 × TIR), has been set with the power programsprovided for its subset as described in Table 1. At the end of thereaction, the mixture was filtered, diluted with ethanol (2 mL)and left under vigorous stirring for 30 minutes at 50 °C. Themixture was then evaporated under reduced pressure and asmall amount of a saturated solution of sodium bicarbonate(3.8 mL, 10 mmol NaHCO3) was added. After the evolution ofCO2, the precipitation of the peracetylated product was observed. The products were separated by simple decantation. Forcompounds which do not precipitate upon addition of NaHCO3,an extraction with AcOEt was needed. The organic phase, afterdrying with Na2SO4, filtration and evaporation, gave the reaction crude.
References:
Oliverio, Manuela;Costanzo, Paola;Nardi, Monica;Calandruccio, Carla;Salerno, Raffaele;Procopio, Antonio [Beilstein Journal of Organic Chemistry,2016,vol. 12,p. 2222 - 2233] Location in patent:supporting information
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