HRID531448

反应详情

EQUATION

反应方程式

HRID 531448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 5-bromo-6-cyclopropyl-2-(trimethylsilyl)-1H-pyrrolo[2,3-b]pyridine (1.5 g, 4.84 mmol), tert-butanol (15 mL), 9N-hydrochloric acid (15 mL) was heated to reflux for 8 hours. Reaction mixture was cooled and basified with 50% sodium hydroxide to pH 8, extracted with ethyl acetate. Organic portion was in turn washed with brine, dried over sodium sulfate and concentrated to give 910 mg (79.13% yield) of the title compound. 1H NMR (CDCl3, 300 MHz) δ 9.43 (bs, 1H), 8.06 (s, 1H), 6.39-6.38 (m, 1H), 2.647-2.603 (m, 1H), 1.09-1 (m, 4H). LCMS: m/z=237.0 (M+1).

WORKUP

后处理

  1. temperatureto reflux for 8 hours
  2. customReaction mixture
  3. temperaturewas cooled
  4. extractionextracted with ethyl acetate
  5. washwashed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated