HRID1961473
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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
2-Amino-5-bromonicotinaldehyde (0.50 g, 2.49 mmol) and N-(4-tert-butylbenzyl)-3-oxobutanamide (0.62 g, 2.49 mmol) were suspended in piperidine (1.0 ml) and EtOH (1.0 ml) in a high-pressure vial. The mixture was heated at 120° C. for 4.5 hours and then cooled to room temperature. The reaction was diluted with water (40 ml) and extracted with CH2Cl2 (3*30 ml). Combined organics were washed with water (30 ml), dried over MgSO4 and evaporated. The crude product was purified by flash chromatography using CH2Cl2/CH3OH (20:1) as eluent to give 0.56 g (54%) of 6-bromo-N-(4-tert-butylbenzyl)-2-methyl-1,8-naphthyridine-3-carboxamide as yellow solids.
WORKUP
后处理
- temperaturecooled to room temperature
- extractionextracted with CH2Cl2 (3*30 ml)
- washCombined organics were washed with water (30 ml)
- dry with materialdried over MgSO4
- customevaporated
- customThe crude product was purified by flash chromatography