These common heterocyclic compound, 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. category: bromides-buliding-blocks
To a 250 ml three-mouth bottle adding 5.04g (0.022 muM) precursor 1 (through the implementation of example one preparation) and 3.26g (0.01 muM) 2, 8 – dibromodiphenyl benzofuran, the mixture thus obtained is VI, VI is added to the mixture in the 40g toluene. Opening stirring, system for the picture and the turbid, N2Replacement system 10min. In the system by adding 2.8g (0.025 muM) tert-butanolate, 0.18g (2 × 10-4Mol) Pd2(Dba)3And 0.12g (4 × 10-4Mol) tri-butyl phosphine four fluoroborates, 80 C reaction 8 hours. The said technological, cooling to 20 – 25 C, the reaction liquid filtration, filtrate directly filtering of the silica gel column, eluting with toluene, the solvent under reduced pressure, to be brownish red color oil of 6.5g. In the above-mentioned crude product in adding toluene and hexane recrystallization (mass ratio of 2:1), vacuum drying oven drying 3h, gain the light yellow powder 2.5g, yield: 40.2%.
The synthetic route of 2,8-Dibromodibenzo[b,d]furan has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CECEP Wanrun Co., Ltd.; Ren Huicai; Pang Maoyin; Yang Fushan; Tian Shaozhen; Shi Rujin; Hu Baohua; (14 pag.)CN105153085; (2017); B;,
Bromide – Wikipedia,
bromide – Wiktionary