HRID1878184

反应详情

EQUATION

反应方程式

HRID 1878184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 2-(2,4-dimethoxybenzylamino)-6-fluoro-3-methoxyquinoxaline (2.70 g, 7.86 mmol), 60 ml of 50% trifluoroacetic acid in dichloromethane was added at room temperature. The resulting mixture was stirred at room temperature for 24 hours and concentrated under the reduced pressure to remove the solvent. The residue was neutralized with saturated sodium bicarbonate solution and then NaCl solution was added thereto. The product was extracted with dichloromethanee and the organic layer was dried over MgSO4. After concentration under the reduced pressure, the crude product was purified by SiO2 column chromatography. Extraction of the residue with a n-hexane:ethyl acetate (4:1) mixture and concentration gave 1.27 g of the titled compound (yield, 84%).

WORKUP

后处理

  1. concentrationconcentrated under the reduced pressure
  2. customto remove the solvent
  3. additionNaCl solution was added
  4. extractionThe product was extracted with dichloromethanee
  5. dry with materialthe organic layer was dried over MgSO4
  6. concentrationAfter concentration under the reduced pressure
  7. customthe crude product was purified by SiO2 column chromatography
  8. extractionExtraction of the residue
  9. concentrationwith a n-hexane:ethyl acetate (4:1) mixture and concentration