Synthetic Route of 38573-88-5, The chemical industry reduces the impact on the environment during synthesis 38573-88-5, name is 1-Bromo-2,3-difluorobenzene, I believe this compound will play a more active role in future production and life.
Then 2,3-difluorobromobenzene (T-10) (115.2 g) was dissolved in DryTHF (600 ml), and the resultant solution was cooled to -70°C. In a nitrogen atmosphere, n-BuLi (364 ml) was added dropwise, and agitation was carried out at -70°C for 2 hours. Then, a DryTHF solution of cyclohexanedione monoethylene ketal (T-3) (93.6 g) was slowly added dropwise at -70°C, and the resultant solution was heated to room temperature and agitated for 16 hours. After completion of the reaction, 2N-HCl (200 ml) was added, extraction was carried out with toluene, an organic layer was washed with water and a saturated aqueous solution of sodium chloride, and then the resultant solution was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and thus a light brown solid was obtained. The resultant material was dissolved in toluene (400 ml), p-TsOH (4.74 g) was added, and heating reflux was carried out for 4 hours while performing dehydration. After completion of the reaction, extraction was carried out with toluene, an organic layer was washed with water and a saturated aqueous solution of sodium chloride, and then the resultant solution was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and thus a light brown solid was obtained. The resultant material was subjected to silica gel column chromatography (heptane:ethyl acetate = 20:1 in a volume ratio) and recrystallization (Solmix), and thus (T-11) was obtained as a colorless crystal (121.0 g, yield: 80percent).
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, 1-Bromo-2,3-difluorobenzene, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; JNC Corporation; JNC Petrochemical Corporation; EP2484658; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary