HRID2375942

反应详情

EQUATION

反应方程式

HRID 2375942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customIPA was evaporated at 35° C.
  2. additionwater was added to the residue
  3. customThe precipitate formed
  4. filtrationwas filtered
  5. washwashed with water
  6. customdried under vacuum