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 3-(2-chloroethoxy)-5-methyl-1-(6-methoxynaphthalen-2-yl)-1H-pyrazol (0.63 g, 2 mmol) and morpholine (0.96 g, 8 mmol) in dimethylformamide (10 ml) was heated to 95° C., in a nitrogen atmosphere, during 20 hrs. Next, it was cooled, the DMF was evaporated in a rotavapor and water and dichloromethane was added to the residue. The organic phase was washed with water and, subsequently, it was extracted with HCl 2N several times. The collection of acidic waters was basified by the addition of NaOH 20% and it was extracted with dichloromethane, which was dried over Na2SO4, filtered and evaporated, thereby leaving a residue of 448 mg of 4-{2-[1-(6-methoxynaphthalen-2-yl)-5-methyl-1H-pyrazol-3-yloxy]ethyl}morpholine (yield: 61%) in the form of a colourless oil.
WORKUP
后处理
- temperatureNext, it was cooled
- customthe DMF was evaporated in a rotavapor and water and dichloromethane
- additionwas added to the residue
- washThe organic phase was washed with water
- extractionsubsequently, it was extracted with HCl 2N several times
- customThe collection of acidic waters
- additionwas basified by the addition of NaOH 20% and it
- extractionwas extracted with dichloromethane, which
- dry with materialwas dried over Na2SO4
- filtrationfiltered
- customevaporated