反応 #814097

反応方程式

ethyl acetate

methyl 3-iodobenzoate

3-nitrophenol

K2CO3

→

product

3-[(3-carbomethoxyphenyl)oxy]nitrobenzene

溶媒

water

pyridine

反応条件

後処理

1. 1
   温度the reaction mixture was heated to reflux
2. 2
   洗浄The organic layer was washed twice with 10% aq. HCl solution
3. 3
   その他The solution was dried (Na2 SO4)
4. 4
   ろ過filtered
5. 5
   濃縮concentrated in vacuo
6. 6
   その他to provide the crude product
7. 7
   その他Purification by silica gel chromatography (CH2Cl2)

実験手順

A solution of methyl 3-iodobenzoate (2.54 g), 3-nitrophenol (1.48 g), and K2CO3 (3.97 g) in 60 mL of pyridine was warmed to 100° C. under nitrogen atmosphere. Copper powder (1.84 g) was added, and the reaction mixture was heated to reflux. After 22 h, The reaction was cooled to room temperature and poured into ethyl acetate and water. The organic layer was washed twice with 10% aq. HCl solution, then with sat. aq. NaHCO3 solution, then with brine. The solution was dried (Na2 SO4), filtered, and concentrated in vacuo to provide the crude product. Purification by silica gel chromatography (CH2Cl2) provided the product as a yellow oil.

出典