HRID2375942
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 5-bromo-4-chloro-1-triisopropylsilanyl-1H-pyrrolo[2,3-b]pyridine (10.1 g, ≈14.0 mmol; crude material prepared according to Tetrahedron Lett., 2004, 45, 2317-2319) in IPA (250 mL) at 0° C. was added 2N H2SO4 (25 mL) and the mixture was allowed to warm to RT and stirred overnight. IPA was evaporated at 35° C. and water was added to the residue and neutralized with 2N NaOH. The precipitate formed was filtered, washed with water followed by hexane, and dried under vacuum to yield the title compound as off-white solid. MS (ES+): m/z 233.01 (100) [MH+]; HPLC: tR=4.51 min (ZQ2000, polar—15 min).
WORKUP
后处理
- customIPA was evaporated at 35° C.
- additionwater was added to the residue
- customThe precipitate formed
- filtrationwas filtered
- washwashed with water
- customdried under vacuum