反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
The process according to claim 4, wherein 2-chloro-N-(2-chloro-4-methyl-3-pyridyl)-3-pyridine carboxamide is heated with cyclopropylamine in the presence of 1 to 2 mol of calcium oxide in diglyme to 135° to 145° C. for 6 to 7 hours, the reaction mixture is then cooled down to 20° to 30° C. and filtered, the filter cake is washed with diglyme and the combined filtrates are concentrated, the residue is then diluted with diglyme and this solution is added to a solution or suspension of sodium hydride in diglyme, heated to 130° to 140° C., and the reaction mixture is kept at a temperature of 130° to 140° C. for 30 minutes to one hour and then the reaction medium is distilled off, the residue is hydrolysed at a temperature of 50° to 80° C. and then cooled to a temperature of about 25° C. and mixed with an inert solvent and an organic acid and the reaction mixture is stirred for about 1 hour at 10° to 25° C., the resultant suspension of the product is separated, washed with an inert solvent, followed by water and alcohol to give nevirapine.
WORKUP
后处理
- temperaturethe reaction mixture is then cooled down to 20° to 30° C.
- filtrationfiltered
- washthe filter cake is washed with diglyme
- concentrationthe combined filtrates are concentrated
- additionthe residue is then diluted with diglyme
- additionthis solution is added to a solution or suspension of sodium hydride in diglyme
- temperatureheated to 130° to 140° C.
- waitthe reaction mixture is kept at a temperature of 130° to 140° C. for 30 minutes to one hour
- distillationthe reaction medium is distilled off
- customis hydrolysed at a temperature of 50° to 80° C.
- additionmixed with an inert solvent
- additionthe resultant suspension of the product
- customis separated
- washwashed with an inert solvent