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ChemicalBook CAS DataBase List 4-BROMODIBENZOTHIOPHENE
97511-05-2

4-BROMODIBENZOTHIOPHENE synthesis

3synthesis methods
Dibenzothiophene

132-65-0

4-BROMODIBENZOTHIOPHENE

97511-05-2

The general procedure for the synthesis of 4-bromodibenzothiophene from dibenzothiophene: Dibenzothiophene was dissolved in tetrahydrofuran (THF) at -40°C, and 2.5 M n-butyllithium (n-BuLi) solution was slowly added and reacted for 1 hour. Subsequently, the temperature of the reaction mixture was raised to 0 °C and 1,2-dibromoethane was slowly added dropwise at -78 °C. After completion of the dropwise addition, the reaction mixture was gradually warmed to room temperature and stirred for 12 hours. Upon completion of the reaction, the solvent was removed by reduced pressure distillation and the residue was separated by extraction with water and chloromethane (MC). The organic phase was collected, concentrated and recrystallized from chloromethane (MC) and hexane to give a white solid intermediate in 95% yield.

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Yield:97511-05-2 95%

Reaction Conditions:

Stage #1: dibenzothiophenewith n-butyllithium in tetrahydrofuran at -40 - 0; for 7 h;
Stage #2: with ethylene dibromide in tetrahydrofuran at -78 - 20; for 12 h;

Steps:

3 Synthesis of (Dibenzothiophene) sub-unit pen trillion mote five pen die method

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 95%.

References:

KR101578475,2015,B1 Location in patent:Paragraph 0090; 0091; 0092; 0093; 0095

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