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With copper(l) iodide; potassium carbonate; cis-N,N'-dimethyl-1,2-diaminocyclohexane; In N,N-dimethyl-formamide; at 120℃; for 0.666667h;Microwave irradiation;
Step 1 : A mixture of A-24.1 (2.00 g, 1 1 .0 mmol), A-24.2 (3.80 g, 17.0 mmol), Cul (0.13 g, 0.68 mmol), A-24.3 (0.14 mL, 1 .00 mmol) and K2C03 (2.30 g, 17.0 mmol) in dry DMF (10 mL) is heated to 120°C by microwave irradiation and stirred for 40 min. The mixture is poured into water and extracted with Et20. The aq. phase is acidified with HCI (4N aq. solution) and extracted with EA. The combined organic phases are dried and concentrated to give the crude product which is purified by flash column chromatography on silica gel (using a solvent gradient from 100percent EA to EA/MeOH = 9/1 ) to provide 3.6 g of A-24.4. APCI+/-: 365 [M+H]+; HPLC (Rt): 1 .10 min (Method N).
With copper(l) iodide; potassium carbonate; cis-N,N'-dimethyl-1,2-diaminocyclohexane; In N,N-dimethyl-formamide; at 120℃; for 0.666667h;Microwave irradiation;
Step 1 : A mixture of A-21.1 (2.00 g, 1 1 .0 mmol), A-21.2 (3.88 g, 17.1 mmol), Cul (0.13 g, 0.68 mmol), A-21.3 (0.15 mL, 1 .03 mmol) and K2C03 (2.36 g, 17.1 mmol) in dry DMF (10 mL) is heated to 120°C by microwave for 40 min. The mixture is poured into water and extracted with Et20. The aq. phase is acidified with HCI (4M aq. solution) and extracted with EA. The combined organic phases are dried and concentrated to give the crude product which is purified by flash column chromatography on silica gel (using a solvent gradient from 100percent EA to EA/MeOH = 9/1 ) to provide 3.6 g of A-21.4. APCI+/-: 365 [M+H]+; HPLC (Rt): 1.10 min (method (0304) N).
3.6 g
With copper(l) iodide; potassium carbonate; cis-N,N'-dimethyl-1,2-diaminocyclohexane; In N,N-dimethyl-formamide; at 120℃; for 0.666667h;
A mixture of A-6.1 (2.00 g, 11.0 mmol), A-6.2 (3.88 g, 17.1 mmol), Cul (0.13 g, 0.68 mmol), A-6.3 (0.15 mL, 1.03 mmol) and K2003 (2.36 g, 17.1 mmol) in dry DMF (10 mL) isheated to 12000 by microwave for 40 mm. The mixture is poured into water and extracted with Et20. The aq. phase is acidified with HCI (4M aq. solution) and extracted with EA. The combined organic phases are dried and concentrated to give the crude product which is purified by flash column chromatography on silica gel (using a solvent gradient from 100percent EA to EAIMeOH = 9/1) to provide 3.6 g of A-6.4. APCI+/-: 365 [M+H] HPLC (Rt): 1.10 mm (methodG).
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