Synthetic Route of 103-64-0, A common heterocyclic compound, 103-64-0, name is (2-Bromovinyl)benzene, molecular formula is C8H7Br, 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.
To a solution of an appropriate amount of an organic solvent (a mixture of N, N-dimethylformamide (DMF) and polyethylene glycol 200 (PEG-200) in a volume ratio of 4: 1)100 mmol of the compound of the above formula (I), 60 mmol of the compound of the above formula (II), 8 mmol of catalyst bis (triphenylphosphine) cyclopentadienyl ruthenium chloride, 120 mmol of an oxidizing agent bis (trifluoroacetic acid) iodobenzene (PhI (TFA) 2),15 mmol of organic ligands L1, 80 mmol of base, 5,7-triazabicyclo [4.4.0] dec-5-ene (TBD) and 8 mmol of activator of niobium pentachloride were added and then stirred to a temperature of 80 C, The reaction was stirred at this temperature for 11 hours;After completion of the reaction, the reaction system is naturally cooled to room temperature and the pH is adjusted to neutral, filtered and the filtrate is saturated Washed with brine and extracted with ethyl acetate 2-3 times. The combined organic phases were dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was passed through Silica gel column chromatography eluting with a 1: 2 by volume mixture of chloroform and petroleum ether to give a compound of the above formula (III) The yield was 89.7%.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Huang Cheng; Bu Gonggaofamingren; (11 pag.)CN106278838; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary