HRID523024

反应详情

EQUATION

反应方程式

HRID 523024 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred solution of 5-bromo-6-chloro-3-trimethylsilanylethynyl-pyrazin-2-ylamine (2.0 g, 6.58 mmol) in THF (28 mL) was added a 1 M solution of KOtBu in THF (7.24 mL, 7.24 mmol) slowly at 0° C. under a nitrogen atmosphere. The reaction mixture was stirred at 0° C. for 10 min and then warmed to room temperature. After 2 h, the mixture was concentrated in vacuo and the residue obtained was suspended in water (7.5 mL) and saturated aqueous NaHCO3 (7.5 mL) and stirred overnight at room temperature The solid was filtered, washed with water and hexanes then dried in an oven at 80° C. to give 2-bromo-3-chloro-5H-pyrrolo[2,3-b]pyrazine (1.64 g) as brown solid. LC-MS: 232 (M−H). This was used directly without further purification.

WORKUP

后处理

  1. temperaturewarmed to room temperature
  2. waitAfter 2 h
  3. concentrationthe mixture was concentrated in vacuo
  4. customthe residue obtained
  5. filtrationwas filtered
  6. washwashed with water and hexanes
  7. customthen dried in an oven at 80° C.