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With potassium phosphate; copper(l) iodide; (S,S)-1,2-diaminocyclohexane; In 1,4-dioxane; for 24h;Reflux;
2-bromodibenzo [b, d] thiophene 5.0g (19.0 mM), 7,7-dimethyl-5,7-dihydroindeno [2,1-b] carbazole4.5 g (15.8 mM), CuI 3.0g (15.8 mM),Trans-1,2-diaminocyclohexane1.9 mL (15.8 mM)And 3.3 g (31.6 mM) of K3PO4 Dioxane and then refluxed for 24 hours. After the reaction was completed, distilled water and DCM were added at room temperature and extracted. The organic layer was dried with MgSO 4 and the solvent was removed using a rotary evaporator. The reaction product was purified by column chromatography (DCM: Hex = 1: 3) and recrystallized from methanol to obtain 7.3 g (85%) of the target compound 8-2.
85%
With potassium phosphate; copper(l) iodide; (S,S)-1,2-diaminocyclohexane; In 1,4-dioxane; for 24h;Reflux;
1) Preparation of compound 10-2 5.0 g (19.0 mmol) of 2-bromodibenzo [b, d] thiophene, 7,7-dimethyl-5,7-dihydroindeno [2,1-b] carbazole 4.5 g (15.8 mmol) of CuI 3.0g (15.8 mmol), Trans-1, 2-diaminocyclohexane (1.9 mL, 15.8 mmol) and 3.3 g (31.6 mmol) of K3PO4 was dissolved in 100 mL of 1,4-oxalic acid and refluxed for 24 hours. After the reaction was completed, distilled water and DCM were added at room temperature and extracted. The organic layer was dried with MgSO 4 and the solvent was removed using a rotary evaporator. The reaction product was purified by column chromatography (DCM: Hex = 1: 3) and recrystallized from methanol to obtain 7.3 g (85%) of the target compound 10-2.
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