反応 #1973968

反応方程式

2,4,6-triiodophenol

trimethylsilyldiazomethane

methanol

→

1,3,5-triiodo-2-methoxybenzene

溶媒

MTBE

反応条件

後処理

1. 1
   その他to give a yellow solution
2. 2
   温度The solution was cooled in an ice bath
3. 3
   その他resulting in calm bubbling
4. 4
   その他The vessel was sealed
5. 5
   その他The reaction solution was partitioned between EtOAc and water
6. 6
   洗浄the organic layer was washed with 1M HCl, saturated NaHCO3, and saturated NaCl
7. 7
   乾燥The EtOAc was dried (MgSO4)
8. 8
   ろ過filtered
9. 9
   濃縮concentrated
10. 10
    その他to give a tan solid that
11. 11
    その他was used without purification (4.8 g, 94%)

実験手順

In a 250 mL pressure vessel was added 2,4,6-triiodophenol (5 g, 10.60 mmol) in MTBE (60 ml) to give a yellow solution. The solution was cooled in an ice bath and 2.0M trimethylsilyldiazomethane (7.95 ml, 15.90 mmol) was added at a fast drip followed by dropwise addition of methanol (6 mL) resulting in calm bubbling. The vessel was sealed and stirred at room temperature for 4 h. The reaction solution was partitioned between EtOAc and water and the organic layer was washed with 1M HCl, saturated NaHCO3, and saturated NaCl. The EtOAc was dried (MgSO4), filtered and concentrated to give a tan solid that was used without purification (4.8 g, 94%).

出典