HRID987542
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
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
- temperatureat reflux for 1 h
- filtrationfiltered through celite
- concentrationthe filtrate concentrated
- additionAqueous NH4OH (11% in H2O, 45 mL) was added to the residue
- extractionthe solution was extracted with CH2Cl2 (3×30 mL)
- dry with materialThe combined organics were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated