反应 #42461

ord-c1dd2980181a479f9a861aa29f4deeb3

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling to room temperature
  2. 2
    workup.STIRRINGstirred for 30 min
  3. 3
    过滤The mixture was filtered
  4. 4
    洗涤washed with water and hexanes
  5. 5
    过滤The yellow powder was collected by filtration
  6. 6
    其他dried in vacuum oven overnight

实验过程

To a solution of methyl 4-hydroxy-3-nitrobenzoate (2.0 g) in acetic acid (15 mL) was added iodine monochloride (1.65 mg) in acetic acid, and the mixture was stirred at 100° C. for 1.5 h. After cooling to room temperature, the mixture was poured into water (200 mL), and stirred for 30 min. The mixture was filtered and washed with water and hexanes. The yellow powder was collected by filtration and dried in vacuum oven overnight to give 2.99 g of the title compound: 1H NMR (300 MHz, CDCl3) δ 11.68, 8.81, 8.72, 3.96.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727997B2uspto-grants-2010_06