反应 #1543069

ord-90c627adde5740e3850db01d5d3c9cd5

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction mixture was evaporated
  2. 2
    workup.ADDITIONwater (5 mL) was added
  3. 3
    过滤the precipitate was filtered
  4. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05843937uspto-grants-1998_12