反应 #1543069
ord-90c627adde5740e3850db01d5d3c9cd5
反应方程式
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他The reaction mixture was evaporated
- 2workup.ADDITIONwater (5 mL) was added
- 3过滤the precipitate was filtered
- 4洗涤washed with water
实验过程
3N NaOH (2 mL) was added to a solution of 3 (250 mg, 1.02 mmol) in methanol (7 mL) and the reaction mixture was stirred overnight at room temperature. The reaction mixture was evaporated and water (5 mL) was added. The solution was neutralized to pH 2 using 20% HCl and the precipitate was filtered and washed with water. 4 was obtained as a grey powder (158 mg, 71% yield), mp: 260° C. (dec). 1H NMR (DMSO-d6, ppm): 11.62 (s, 1 H, NH), 9.77 (s, 1 H, NH), 7.98-7.97 (d, 1 H, J=1.4 Hz, Ar--H), 7.36-7.28 (m, 2 H, Ar--H), 7.02 (d, 1 H, J=1.5 Hz, Ar--H), 2.03 (s, 3 H, CH3CO), Anal. (C11H10N2O3 0.6H2O), C, H, N.