反应详情

温度

150 °C

A mixture of 12 g of 1c and 27 g of ammonium acetate was heated at 150° C. for 14 hours. After cooling to room temperature aqueous 3N NaOH was added and the mixture was extracted with ethyl acetate. The ethyl acetate extract was washed with brine and aqueous 2N hydrochloric acid was added until pH2-3. The acid aqueous layer was separated, made basic (pH10) with aqueous 2N NaOH and extracted with ethyl acetate. The ethyl acetate layer was washed with brine, dried (MgSO4) and concentrated to give 6.4 g of 1d. 1H-NMR 200 MHz (CDCl3) δ: 5.1 (2H, br s), 6.96 (1H, dd, J=6 Hz and J=1 Hz), 7.54-7.70 (2H, m), 7.88 (1H, d, J=2 Hz), 7.98 (1H, d J=6 Hz).

1. additionwas added
2. extractionthe mixture was extracted with ethyl acetate
3. extractionThe ethyl acetate extract
4. washwas washed with brine and aqueous 2N hydrochloric acid
5. additionwas added until pH2-3
6. customThe acid aqueous layer was separated
7. extractionextracted with ethyl acetate
8. washThe ethyl acetate layer was washed with brine
9. dry with materialdried (MgSO4)
10. concentrationconcentrated