반응 #42461

ord-c1dd2980181a479f9a861aa29f4deeb3

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling to room temperature
  2. 2
    workup.STIRRINGstirred for 30 min
  3. 3
    여과The mixture was filtered
  4. 4
    세척washed with water and hexanes
  5. 5
    여과The yellow powder was collected by filtration
  6. 6
    기타dried in vacuum oven overnight

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07727997B2uspto-grants-2010_06