تفاعل #42461

معادلة التفاعل

methyl 4-hydroxy-3-nitrobenzoate

iodine monochloride

water

→

title compound

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

المذيبات

acetic acid

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling to room temperature
2. 2
   workup.STIRRINGstirred for 30 min
3. 3
   ترشيحThe mixture was filtered
4. 4
   غسيلwashed with water and hexanes
5. 5
   ترشيحThe yellow powder was collected by filtration
6. 6
   أخرىdried in vacuum oven overnight

الإجراء التجريبي

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.

المصدر