5,10,15,20-tetra(3,4,5-trimethoxyphenyl)-21H,23H-porphyrin synthesis

Yield:74684-35-8 53%

Reaction Conditions:

with oxygen;acetic acid at 150; under 3750.38 Torr; for 1.9 h;

Steps:

3 Example 3

Dissolving 119g of 3,4,5-trimethoxybenzaldehyde in a 3L pressure-resistant reactor containing 2.5L of acetic acid solution, and raising the temperature to 150 ° C;An oxygen-containing gas (80% oxygen content) is passed from the bottom of the reactor to the reactor.Control the pressure at 0.5 MPa;42 mL of pyrrole was added dropwise to the reactor within 0.5 h, and after 1.4 h of reaction, the reaction was stopped by cooling to 20 ° C;After cooling, the oxygen-containing gas was released to the gas storage tank, and the reaction product obtained in the reactor was filtered to obtain a filter cake. The filter cake was washed with 1.0 L of methanol, and then the filter cake was washed with 0.4 L of hot water, and dried to obtain 77.0 g of a product. . The filtrate obtained by filtration can be recovered by atmospheric distillation to be used.The product was characterized according to the detection method of Example 1, and the results showed that the obtained product was of the formula (1) wherein R1, R2 and R3 were -OCH3. The product yield and purity were tested according to the test method of Example 1, and the results showed that the product yield was 53.0% and the purity was 99.4%.

References:

CN109824679,2019,A Location in patent:Paragraph 0066-0069