HRID453262

反应详情

EQUATION

反应方程式

HRID 453262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureNext, it was cooled
  2. customthe DMF was evaporated in a rotavapor and water and dichloromethane
  3. additionwas added to the residue
  4. washThe organic phase was washed with water
  5. extractionsubsequently, it was extracted with HCl 2N several times
  6. customThe collection of acidic waters
  7. additionwas basified by the addition of NaOH 20% and it
  8. extractionwas extracted with dichloromethane, which
  9. dry with materialwas dried over Na2SO4
  10. filtrationfiltered
  11. customevaporated