反应详情

温度

70 °C

To a solution of iii (0.90 g, 2.74 mmol) in MeOH (25 mL) was added a solution of NaOH (0.55 g, 13.70 mmol) in H2O (5 mL). The resulting solution was heated at 70° C. for 3-4 h then cooled to RT and the solvent removed in vacuo. Water was added to the residue and this mixture extracted with EtOAc (2×50 mL). The organic layer was discarded, and the aqueous portion was carefully acidified (under ice-cooling) with 6N HCl till pH 5. The resulting precipitate was filtered, washed with ice-cold water and ether. The off-white solid thus obtained was dried under high vacuum to obtain compound iv (0.70 g, 85%). 1H-NMR (400 MHz, DMSO-d6): δ10.60 (br s, 1H), 9.07 (br s, 1H), 8.55 (s, 1H), 8.0 (br s, 1H), 7.13-7.42 (m, 6H), 3.12 (m, 2H), 1.05 (t, J=7.20 Hz, 3H); [M+H]+ m/z=301.21.

1. temperaturethen cooled to RT
2. customthe solvent removed in vacuo
3. additionWater was added to the residue
4. extractionthis mixture extracted with EtOAc (2×50 mL)
5. temperature(under ice-cooling) with 6N HCl till pH 5
6. filtrationThe resulting precipitate was filtered
7. washwashed with ice-cold water and ether
8. customThe off-white solid thus obtained
9. customwas dried under high vacuum