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
4.4 ml (26.4 mmol) of 6N aqueous sodium hydroxide solution are added to 0.5 g (1.7 mmol) of 3-(4-amino-3-methoxybenzoyl)imidazo[1,5-a]pyridine-1-carbonitrile obtained in example 85 in 50 ml of ethanol under a nitrogen atmosphere. After heating at reflux for 2 hours, the reaction medium is concentrated under reduced pressure. The residue obtained is washed with water, with acetone and with ethyl ether and then dried. 0.447 g of a yellow solid is collected. The product is salified by addition of a 1N solution of hydrochloric acid in ethyl ether. 0.310 g of a yellow solid is obtained. Melting point: 241° C.; 1H NMR (d6-DMSO): 3.89 (3H, s), 6.74 (1H, d), 7.24-7.27 (1H, m), 7.45-7.49 (1H, m), 7.88 (1H, s), 8.33 (1H, d), 8.42 (1H, d), 9.65 (1H, d)
WORKUP
后处理
- temperatureAfter heating
- temperatureat reflux for 2 hours
- concentrationthe reaction medium is concentrated under reduced pressure
- customThe residue obtained
- washis washed with water, with acetone and with ethyl ether
- customdried
- custom0.447 g of a yellow solid is collected
- additionThe product is salified by addition of a 1N solution of hydrochloric acid in ethyl ether