反应详情

To a screw-cap test tube are added copper(I) iodide (23.74 mg, 0.125 mmol), 2-chloro-4,4-difluoro-1′-[(3-methyl-1H-pyrazol-4-yl)methyl]spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine] (233.00 mg, 0.623 mmol), potassium carbonate (182.71 mg, 1.31 mmol), toluene (2 mL) (previously bubbled with nitrogen for 20 min) and a stir bar. The reaction mixture is bubbled with nitrogen for 20 minutes and then 2-iodo-3-methoxypyridine (302.01 mg, 1.25 mmol) and trans-N,N′-dimethylcyclohexane-1,2-diamine (39.31 mL, 0.25 mmol) are added. The reaction tube is quickly sealed (caution: build-up of pressure possible; use a safety shield) and immersed in a preheated oil bath at 110° C. for 24 hours with the aid of a magnetic stirrer. Then, the mixture is poured on SCX column (25 g) and eluted with methanol and then 2N solution of ammonia in methanol. The basic fraction is concentrated and the resulting residue is purified by basic-HPLC to give 162 mg of the title compound. MS (m/z): 481 (M+1).

1. custompreviously bubbled with nitrogen for 20 min) and a stir bar
2. customThe reaction mixture is bubbled with nitrogen for 20 minutes
3. customThe reaction tube is quickly sealed (caution
4. additionThen, the mixture is poured on SCX column (25 g)
5. washeluted with methanol
6. concentrationThe basic fraction is concentrated
7. customthe resulting residue is purified by basic-HPLC