反应详情

A mixture of methyl 2-azidoacetate, 4-benzyloxy-3-fluoro-benzaldehyde and sodium methanolate (in methanol) in toluene was reacted for 3 h at 0° C. The residue after filtration of the suspension was washed with methanol, partitioned between ethyl acetate and ammonium chloride solution and extracted with ethyl acetate. The combined organic layers were dried with Na2SO4, evaporated to dryness and the residue taken up in p-xylene and brought to reflux temperature for 2 h. After concentration the mixture was left to crystallize and the formed crystals were filtered off and washed with toluene. The title compound was after drying at 40° C. under vacuum obtained as yellow crystals. MS (m/e): 300.3 (MH+, 100%).

1. customwas reacted for 3 h at 0° C
2. filtrationThe residue after filtration of the suspension
3. washwas washed with methanol
4. custompartitioned between ethyl acetate and ammonium chloride solution
5. extractionextracted with ethyl acetate
6. dry with materialThe combined organic layers were dried with Na2SO4
7. customevaporated to dryness
8. temperatureto reflux temperature for 2 h
9. concentrationAfter concentration the mixture
10. waitwas left
11. customto crystallize
12. filtrationthe formed crystals were filtered off
13. washwashed with toluene
14. customafter drying at 40° C. under vacuum
15. customobtained as yellow crystals