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ChemicalBook CAS DataBase List 7H-DIBENZO[C,G]CARBAZOLE
194-59-2

7H-DIBENZO[C,G]CARBAZOLE synthesis

11synthesis methods
-

Yield:194-59-2 98%

Reaction Conditions:

with ammonium hydroxide;ammonium bisulfite at 220; for 16 h;Autoclave;Temperature;Reagent/catalyst;

Steps:

1.2 (2) Production by two-step mixing of aminating agentExample 1-8

General procedure: Racemic 2,2'-dihydroxy-1,1'-binaphthyl (rac-BINOL, 1.6 g, 5.6 mmol), half the amount of ammonium sulfite monohydrate (AR, as described in Table 2 as aminating agent 9.0 g, 67 mmol) and aqueous ammonia (12 mL, 174 mmol) were placed in an autoclave. The mixture in the autoclave was stirred at the reaction temperature described in Table 2 for half the reaction time described in Table 2 and the mixture was cooled to 25 ° C. To the cooled reaction mixture, the remaining half amount of AR (9.0 g, 67 mmol) and aqueous ammonia (12 mL, 174 mmol) described in Table 2 were added, and the reaction described in Table 2 was performed again.The mixture was stirred at the temperature for the remaining reaction time described in Table 2.The reaction mixture was cooled to 25 ° C., and the resulting solid was washed with water and filtered. The filtrate was recrystallized with benzene to separate rac-NOBIN and DBC.The reaction yield was calculated from chiral HPLC, and the isolated yield recrystallized from benzene was calculated and described in Table 2.

References:

JP2019/43941,2019,A Location in patent:Paragraph 0048; 0054-0061

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