反应详情

To a solution of 1-benzyl-4-(1-triisopropylsilanyl-1H-indazol-5-yl)-piperazin-2-one (0.78 g, 1.7 mmol) in 8.5 mL THF at −78° C. was added sec-butyllitium (1.3 mL, 1.9 mmol) drop-wise over 5 minutes. After 30 minutes 4-bromomethyl-tetrahydropyran (0.36 g, 2.0 mmol) was added in one portion and mixture was warmed to room temperature. After 18 hours H2O was added and the mixture was extracted with ethyl acetate. The combined organic layerss were washed with H2O, brine, dried over NaSO4, filtered and concentrated in vacuo. Purification via flash chromatography afforded 1-benzyl-3-(tetrahydro-pyran-4-ylmethyl)-4-(1-triisopropylsilanyl-1H-indazol-5-yl)-piperazin-2-one (0.55g, 90%) as a white foam.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe combined organic layerss were washed with H2O, brine
3. dry with materialdried over NaSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification via flash chromatography