反应详情

Methyl 2-(2-methylphenylamino)-5-benzoxazolylacetate (2.32 g, 7.86 mmol) was dissolved in THF (40 ml). After addition of 0.25N NaOH (40 ml) under stirring at room temperature, the mixture was stirred for 15 hours. The residue, which had been obtained by distilling the reaction mixture under reduced pressure to remove the solvent, was acidified with 1N HCl. The crystals thus obtained were collected by filtration under reduced pressure, washed with water, dried under reduced pressure, whereby the title compound (894 mg) was obtained as a pale black crystalline powder. The water layer was extracted with a chloroform/methanol (10/1) mixture. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent, whereby the title compound (1.03 g) was obtained as a colorless solid (total yield: 88%).

1. stirringthe mixture was stirred for 15 hours
2. customThe residue, which had been obtained
3. distillationby distilling the reaction mixture under reduced pressure
4. customto remove the solvent
5. customThe crystals thus obtained
6. filtrationwere collected by filtration under reduced pressure
7. washwashed with water
8. dry with materialdried under reduced pressure, whereby the title compound (894 mg)
9. customwas obtained as a pale black crystalline powder
10. extractionThe water layer was extracted with a chloroform/methanol (10/1) mixture
11. washThe extract was washed with saturated brine
12. dry with materialdried over anhydrous sodium sulfate
13. distillationdistilled under reduced pressure
14. customto remove the solvent, whereby the title compound (1.03 g)
15. customwas obtained as a colorless solid (total yield: 88%)