反应详情

To a stirred mixture of 0.86 g of sodium hydride (50% oil dispersion) in 50 ml of dimethylformamide was added, dropwise, 3.0 g of 3-(1-methyl-4-piperidinyl)-1H-indazole in 15 ml of hot dimethylformamide. The reaction mixture was stirred at ambient temperature for 1 hr and then a solution of 3.33 g of (2-bromoethyl)benzene in 10 ml of dimethylformamide was added dropwise. The reaction mixture was stirred for 21/2 days at ambient temperature, cooled to 0° , and water was added dropwise. The mixture was 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 a saturated hydrogen bromide/ether solution was added dropwise. The resultant solid was recrystallized two times from ethanol to yield 2.0 g (36%) of product, mp 163°-164° C.

1. additionwas added
2. stirringThe reaction mixture was stirred for 21/2 days at ambient temperature
3. temperaturecooled to 0°
4. extractionThe mixture was extracted 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. customThe resultant solid was recrystallized two times from ethanol