HRID987542

反应详情

EQUATION

反应方程式

HRID 987542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5,7-Dibromo-4-methoxy-6-azaindole 36 (680 mg, 2.22 mmol), 5% Pd/C (350 mg, 0.17 mmol) and hydrazine (2.5 mL, 80 mmol) in EtOH was heated at reflux for 1 h. The reaction mixture was allowed to cool to rt, filtered through celite and the filtrate concentrated. Aqueous NH4OH (11% in H2O, 45 mL) was added to the residue and the solution was extracted with CH2Cl2 (3×30 mL). The combined organics were dried (MgSO4), filtered and concentrated to yield 4-methoxy-6-azaindole 37 (290 mg, 1.95 mmol, 88%) as an orange solid.

WORKUP

后处理

  1. temperatureat reflux for 1 h
  2. filtrationfiltered through celite
  3. concentrationthe filtrate concentrated
  4. additionAqueous NH4OH (11% in H2O, 45 mL) was added to the residue
  5. extractionthe solution was extracted with CH2Cl2 (3×30 mL)
  6. dry with materialThe combined organics were dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated