反应详情

6-Methyl-1H-indazol-4-amine hydrochloride (0.5 g, 2.7 mmol), phenylmethyl 3-iodobenzoate (0.9 g, 2.6 mmol), copper (I) iodide (14 mg, 0.07 mmol), potassium carbonate (1.2 g, 8.68 mmol) and trans-N,N′-dimethyl-1,2-cyclohexanediamine (20 mg, 0.14 mmol) were heated together in DMF (5 mL) at reflux overnight. The mixture was poured into water (15 mL) and ethyl acetate was added to dissolve the resulting oil. The suspension was then filtered through celite. The organic phase was separated, combined with a second ethyl acetate extract, washed successively with water and brine and then dried over anhydrous sodium sulphate and evaporated under reduced pressure. The residue was purified by silica gel column chromatography (75 g) eluting with 1 to 5% gradient of ethyl acetate in dichloromethane to give the title compound as a light brown oil (0.3 g).

1. temperatureat reflux overnight
2. additionwas added
3. dissolutionto dissolve the resulting oil
4. filtrationThe suspension was then filtered through celite
5. customThe organic phase was separated
6. extractionextract
7. washwashed successively with water and brine
8. dry with materialdried over anhydrous sodium sulphate
9. customevaporated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (75 g)
11. washeluting with 1 to 5% gradient of ethyl acetate in dichloromethane