反应详情

To a stirred mixture of 1.19 g of sodium hydride (50% oil dispersion) in 65 ml of dimethylformamide was added, dropwise, 4.0 g of 3-(1-methyl-4-piperidinyl)-1H-indazole in 20 ml of hot dimethylformamide. The mixture was stirred for 1 hr at ambient temperature and then 1.40 g of chloromethylcyclopropane in 10 ml of dimethylformamide was added dropwise. The reaction mixture was stirred for 21/2 days at ambient temperature. The reaction mixture was quenched with water, extracted with ethyl acetate, washed with water, dried over anhydrous magnesium sulfate and the solvent was removed in vacuo to yield an oil. The oil was dissolved in ether and saturated hydrogen bromide/ether solution was added dropwise to precipitate a salt. The salt was recrystallized from toluene and ethyl acetate to yield 2.8 g (32%) of product, mp 177°-179° C.

1. additionwas added
2. stirringThe reaction mixture was stirred for 21/2 days at ambient temperature
3. customThe reaction mixture was quenched with water
4. extractionextracted with ethyl acetate
5. washwashed with water
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent was removed in vacuo
8. customto yield an oil
9. customto precipitate a salt
10. customThe salt was recrystallized from toluene and ethyl acetate