반응 #2161223

반응 방정식

porphyrin

pyrrole

4-trimethylsilylethynylbenzaldehyde

methanol

→

porphyrin

수율 12.0%

tetrakis(4-trimethylsilylethynylphenyl)porphyrin

수율 12.0%

용매

propionic acid

반응 조건

후처리

1. 1
   온도The temperature was subsequently increased
2. 2
   온도at reflux for 4 hours
3. 3
   workup.WAITwas then left
4. 4
   기타to crystallize
5. 5
   여과The medium was filtered over sintered glass
6. 6
   세척the product was rinsed with methanol

실험 절차

5.02 g of 4-trimethylsilylethynylbenzaldehyde (25 mmol) were dissolved in 210 ml of propionic acid and then heated to 80° C. 1.72 ml of pyrrole (25 mmol) were subsequently added portionwise over a period of one hour. The temperature was subsequently increased and the mixture was kept at reflux for 4 hours. After a return to ambient temperature, 75 ml of methanol were added to the reaction medium, which was then left to stand for 14 hours in order for the porphyrin to crystallize. The medium was filtered over sintered glass and the product was rinsed with methanol. 2.87 g (3 mmol; yield 12%) of the expected porphyrin (1) were obtained in the form of a purple powder.

출처