反应详情

温度

50 °C

To a mixture of compound 37-m (300 mg, crude) in MeOH (10 mL) was added a solution of 20% KOH (10 mL). The mixture was stirred at 50° C. for 2 h. The reaction mixture was filtered. The filtrate was concentrated and the aqueous solution was extracted with DCM, and acidified by concentrated HCl to adjust to about pH 2-3. The solid was filtered and washed with water to afford compound 37-1 (110 mg, 73% for two steps) as a yellow solid. 1H NMR (300 MHz, DMSO-d6) δ 8.827-8.821 (s, 1H), 8.722 (s, 1H), 8.456-8.431 (m, 1H), 8.103-8.035 (m, 2H), 7.733-7.694 (m, 1H), 7.630 (s, 1H), LC-MS (ESI): 361 [M+H]+.

1. filtrationThe reaction mixture was filtered
2. concentrationThe filtrate was concentrated
3. extractionthe aqueous solution was extracted with DCM
4. filtrationThe solid was filtered
5. washwashed with water