HRID1023946

反应详情

EQUATION

反应方程式

HRID 1023946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[2-(benzyloxy)-4-ethylphenoxy]-3-fluoroaniline (500 mg, 1.48 mmol), K2CO3 (1.23 g, 8.9 mmol) and 3-bromo-1-propanol (410 mg, 2.9 mmol) were taken in dry DMF (2 ml) in a microwave vial and was subjected to microwave at 180° C. for 2 h. The reaction mixture was filtered over celite and the residue washed thouroughly with ethyl acetate. The combined organic fractions including the filtrate were washed with water, brine, dried over Na2SO4 and concentrated. The crude obtained was combined with earlier crude products obtained from a 100 mg and 200 mg batches and purified together by column chromatography over silica gel using 40% ethylacetate in pet ether as eluant to get 400 mg (42.6%) of pure title compound.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered over celite
  2. washthe residue washed thouroughly with ethyl acetate
  3. washwere washed with water, brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customThe crude obtained
  7. customobtained from a 100 mg and 200 mg batches
  8. custompurified together by column chromatography over silica gel using 40% ethylacetate in pet ether as eluant