Cyclamen Aldehyde CAS 103-95-7

Synthesized making use of cuminyl chloride as raw material
Add 174 parts of ethyl malonate to a 10% ethanol option consisting of 68 parts of salt ethoxide, warmth to reflux, and then slowly include 168.5 parts of industrial cuminyl chloride dropwise. When the response ends (the alkalinity disappears), add 1200 parts of 10% salt hydroxide remedy and warmth to reflux for 4 hours. After the ethanol is evaporated, the reactant is acidified with hydrochloric acid, and the resulting cuminylmethylmalonic acid is heated to 185 ° C till no carbon dioxide runs away. The item was fractionated under minimized pressure, and the 153 ~ 157 ° C( 533Pa) portion was collected, which is p-isopropyl-α-methyldihydrocinnic acid including a small amount of ortho by-products, with a return of 90%.
The above item is passed together with formic acid through a response tube with a temperature level controlled at 350 ° C and equipped with MnO2/pumice, and is converted into aldehyde with a return of 80%. The crude product is distilled under reduced pressure, and the 118-120 ° C( 800Pa) fraction is collected to get Cyclamen Aldehyde.
Synthesized using cumine aldehyde as resources
Liquify 10kg of potassium hydroxide in 400kg of ethanol, blend it with cuminaldehyde at 10 ° C, gradually go down 60kg of propionaldehyde right into it while stirring within 2 to 6 hours, and maintain the temperature level at 10 to 15 ° C. Counteract the catalysts with acetic acid, very first evaporate the ethanol under typical pressure, after that boil down under lowered pressure to recover about 45kg of unreacted cumyl aldehyde, and then collect the 152-158 ° C(1200Pa) fraction, which is p-isopropyl-α-methyl Cinnamaldehyde has a refractive index of 1.5860.
Dissolve the above item in ethanol, area it in an autoclave, add 10% mass of reduced nickel or palladium-carbon stimulant, and carry out hydrogenation at 100 ° C. Afterwards, the stimulant is filtered off, the solvent is recovered by distillation under typical pressure, fractionated under decreased pressure, and the 133 ~ 137 ° C (1.2 kPa) portion is gathered, which is Cyclamen Aldehyde.