反応 #42461

反応方程式

methyl 4-hydroxy-3-nitrobenzoate

iodine monochloride

water

→

title compound

Methyl 4-hydroxy-3-iodo-5-nitrobenzoate

溶媒

acetic acid

acetic acid

反応条件

後処理

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

実験手順

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.

出典