反应详情

温度

70 °C

(S)—N-(3-ethynylphenyl)-6-nitro-7-(tetrahydrofuran-3-yloxy)quinazolin-4-amine (4 g, 0.011 mol) and ammonia hydrochloride (2.4 g, 0.045 mol) was mixed in a solution of 150 mL methanol, 75 mL H2O, 50 ml EA, and then was heated to 70° C. Fe (4.8 g, 0.085 mol) was added and the reaction mixture was heated to reflux for 4 hours. The resulting reaction solution was filtered and concentrated under reduced pressure to remove most of solvent. The residue was diluted in 100 mL H2O, extracted with ethyl acetate (3×100 mL), the organic layers were concentrated to give (S)—N4-(3-ethynylphenyl)-7-(tetrahydrofuran-3-yloxy)quinazoline-4,6-diamine as grey solid 1.8 g (48.9% yield).

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 4 hours
3. customThe resulting reaction solution
4. filtrationwas filtered
5. concentrationconcentrated under reduced pressure
6. customto remove most of solvent
7. additionThe residue was diluted in 100 mL H2O
8. extractionextracted with ethyl acetate (3×100 mL)
9. concentrationthe organic layers were concentrated