Extracurricular laboratory: Synthetic route of 453565-55-4

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Fluoroisophthalonitrile, other downstream synthetic routes, hurry up and to see.

Application of 453565-55-4, The chemical industry reduces the impact on the environment during synthesis 453565-55-4, name is 5-Fluoroisophthalonitrile, I believe this compound will play a more active role in future production and life.

3.00 g (9.03 mmol) of 3,3′-9H-biscarbazole and 4.98 g (36.0 mmol) of potassium carbonate were placed in a 200 ml three-necked flask, and the flask was purged with nitrogen. N, N-Dimethylformamide (78.0 ml) was added to the mixture, and the mixture was stirred at room temperature for 2 hours under a nitrogen stream. After adding 2.93 g (18.0 mmol) of 5-fluoroisophthalonitrile into this mixture, the mixture was stirred at 70 C for 20 hours under a nitrogen atmosphere. After the stirring, the solvent in the mixture was removed by distillation under reduced pressure. After removal, 100 ml of chloroform and 50 ml of water were added to this mixture and stirred. After stirring, the mixture was subjected to suction filtration to obtain a filtrate. The obtained aqueous layer of the filtrate and the organic layer were separated, and the organic layer was washed with water. After washing, magnesium sulfate was added to the organic layer and dried. After drying, the mixture was subjected to suction filtration to obtain a filtrate. The obtained filtrate was concentrated and purified by silica gel column chromatography. As the developing solvent, a mixed solvent of chloroform: ethyl acetate = 10: 1 was used first. The resulting fraction was concentrated, and the resulting solid was recrystallized from a mixed solvent of chloroform and methanol to obtain 0.700 g of a pale orange powdery solid as a target product in a yield of 13.3%.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Fluoroisophthalonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KokuritsuDaigakuHojinKyushuDaigaku; Nippon Steel & Sumikin Kagaku Corporation; Li, Bo; Orita, Akihiro; Miyazaki, Hiroshi; Ohterra, Junjo; Nomura, Hiroko; Adachi, Jihaya; (38 pag.)KR2016/34335; (2016); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts