10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Safety of 2,8-Dibromodibenzo[b,d]furan
2.75 g (10 mmol) of 4-phenylaminodibenzothiophene, 1.63 g (5.0 mmol) of 2,8-dibromodibenzofuran, 2.5 g (26 mmol) of sodium t-butoxide in a 50 ml four-necked flask,50 ml of dehydrated toluene was added and nitrogen bubbling was performed for 1 hour. Then, 3460 mg (0.5 mmol) of Pd2 (dba),290 mg (1.0 mmol) of tri-t-butylphosphonium tetrafluoroborate (t-Bu3PH + BF4-) was added, and the mixture was heated under reflux for 53 hours while stirring under a nitrogen stream. The formation of the desired product was confirmed by TLC and MS. The reaction solution was cooled to room temperature, and the organic layer was extracted with toluene, washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated to obtain a brown viscous product. The obtained viscous material was dissolved in 10 ml of toluene and packed in a column. The resultant was directly purified by silica gel column chromatography (developing solvent: toluene / hexane = 1/4) to obtain the desired product.Yield 1.92g, 54%
The synthetic route of 10016-52-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; National University Corporation Yamagata University; Sasabe, Hisahiro; Kido, Junji; Kamata, Takahiro; (21 pag.)JP2019/26556; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary