反应详情

温度

100 °C

0.3 g of the tent-Butyl ester of 4-(4-hydroxyphenyl)-3,4-dihydro-2H-quinoxaline-1-carboxylic acid is placed in 4.6 ml of dimethylformamide under nitrogen. 0.167 g of 2-(chloromethyl)pyrimidine and 0.508 g of potassium carbonate are added. The reaction medium is heated at 100° C. for 4 h. 0.254 g of potassium carbonate is added and heating is maintained for 1 h 30. After hydrolysis, the reaction medium is extracted with ethyl acetate until the aqueous phase has been completely extracted. The organic phases are combined, washed with a saturated aqueous sodium chloride solution, dried over magnesium sulphate and concentrated to dryness. The crude product obtained is chromatographed on silica gel, elution being carried out with a gradient of methanol in dichloromethane varying from 0% to 9/1. 0.095 g of 1-[4-(pyrimidin-2-ylmethoxy)phenyl]-1,2,3,4-tetrahydro-quinoxaline is obtained.

1. temperatureheating
2. temperatureis maintained for 1 h 30
3. customAfter hydrolysis
4. extractionthe reaction medium is extracted with ethyl acetate until the aqueous phase
5. extractionhas been completely extracted
6. washwashed with a saturated aqueous sodium chloride solution
7. dry with materialdried over magnesium sulphate
8. concentrationconcentrated to dryness
9. customThe crude product obtained
10. customis chromatographed on silica gel, elution