4-Bromodibenzothiophene

Light yellow powder

3 known as a raw material of the synthetic intermediates in said 14 shown in the die plate to benzothiophene (Dibenzothiophene) (tetrahydrofolate) (THF) folic acid Tetrahydropyridines of in -40 ° C 2.5M n-BuLi of paste has better mouth feeling and is slowly and the 1 hour or 2000. Then 0 °C 6 and raised from a temperature -78 ° C and re-stirring time 12 time the dropping a 1, 2-chlorobenzene in 2000 at room temperature. Completion after solvent is removed methyl chloride (methyl chloride) (MC) are determined from the extracted area melt to water. The solvent is concentrated and then and the methyl chloride (methyl chloride) (MC) and a hexane are recrystallized 14 a solid white the intermediates obtained at a yield of 95percent.Dibenzothiophene was dissolved in anhydrous THF (tetrahydrofuran), it lowers the temperature of the reaction to -40 °C. n-BuLi (2.5 Min hexane) was slowly added dropwise, and after stirred for 6 hours the reaction at 0°C . Thereafter, the lower the temperature of the reaction to -78 °C, 1, 2-dibromoethane was added dropwise to a solution obtained by dissolving in THF and stirred for 14 hours at room temperature. After the reaction was completed by using a reduced pressure apparatus to remove the volatile organic solvent and extracted with CH2Cl2 and waterIt was clean. After removing a small amount of water over anhydrous MgSO4 and filtered under reduced pressure, the product was produced by concentrating the organic solvent was recrystallized using hexane and CH2Cl2 solvent to give the desired intermediate A (yield: 71percent).[0187] In an argon atmosphere, 48.2 g (261.6 mmol) of dibenzothiophene was added with 480 ml of dehydratedtetrahydrofuran. The resultant mixture was cooled to - 30 °C and added with 164 ml (262.0 mol) a 1.60 M hexane solutionof n-butyllithium dropwise. The temperature was raised to room temperature over one hour under stirring. After stirringat room temperature for 3 h, the mixture was cooled to-60 °C and added with a solution of 73.7 g (393 mmol) of 1, 2-dibromoethane in 50 ml dehydrated tetrahydrofuran dropwise over one hour.[0188] After stirring for 15 h at room temperature, the mixture was poured into 400 ml of iced water and extracted withtoluene. The organic layer was washed with brine, dried over MgSO4, filtered, and then concentrated. The concentratewas purified by silica gel column chromatography. The crude product was recrystallized from heptane several times toobtain 33.1 g of white crystal, which was identified as the following intermediate 1-6 by FD-MS (yield: 48percent).

Molecular Weight:263.15
XLogP3:5.1
Hydrogen Bond Acceptor Count:1
Exact Mass:261.94518
Monoisotopic Mass:261.94518
Topological Polar Surface Area:28.2
Heavy Atom Count:14
Complexity:218
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes