Background and overview[1][2]
The chemical name of cinnamyl formate is phenylpropyl formate and 3-phenyl-2-propen-1-ol formate. It is an important fine chemical intermediate and is widely used in the production of medicines, spices and other products. middle. At present, the general methods for preparing cinnamyl formate mainly include:
1) Formic acid and cinnamyl alcohol are directly esterified to prepare cinnamyl formate. The use of different catalysts (such as ammonium chloride, magnesium chloride, phosphoric acid, concentrated sulfuric acid, etc.) has a greater impact on the yield and product quality of the produced cinnamyl formate. The cinnamyl formate product synthesized by this method has a low yield and poor product quality.
2) Cinnamyl formate is synthesized from the reaction of sodium formate and cinnamyl chloride in the presence of pyridine. Although this synthesis method is relatively simple, it consumes a large amount of solvent. The main raw materials, sodium formate and cinnamyl chloride, have limited sources, and the raw materials and solvents used are expensive, making it uneconomical from an economic perspective.
Preparation[2]
A preparation method of cinnamyl formate (3-phenyl-2-propen-1-ol formate), which method uses formic acid and cinnamyl alcohol in an organic solvent toluene or benzene as a solvent, and phosphoric acid or toluene Sulfonic acid is used as a catalyst to prepare cinnamon formate. The process is simple, the operation is convenient, the raw materials are easily available, the cost is low, the yield is high, and there is no pollution to the environment. It is very suitable for industrial production. The technical solution steps are:
A. Dissolve formic acid in an organic solvent at a mass ratio of 1:1-1.5, add the catalyst at a ratio of 1.5 or 2 or 3 or 4% of the mass of formic acid, stir evenly and cool to 20 or 25 or 30°C, the insulation temperature is controlled at 20 or 22 or 25 or 27 or 30°C, and cinnamyl alcohol is added dropwise. The molar ratio of formic acid to cinnamyl alcohol is 2-5:1.
B. The time for adding cinnamyl alcohol dropwise is 1 or 2 or 3 hours, and the temperature is kept at 20 or 22 or 25 or 27 or 30°C for 0.5 hour or 1 hour. After the dripping of cinnamyl alcohol is completed, it is washed and neutralized with water to obtain cinnamon formate. Crude ester.
C. Reduce the pressure of the crude product to -0.07–0.1Mpa, and control the temperature at 110 or 115 or 120°C to recover the solvent. The solvent recovery is complete.
D. After the solvent is recovered, collect cinnamyl formate (3-phenyl-2- Propylene-1-ol formate) finished product.
Main reference materials
[1] CN200810047359.9 A kind of preparation method of cinnamyl formate
