反应 #1973968

反应方程式

2,4,6-triiodophenol

trimethylsilyldiazomethane

methanol

→

1,3,5-triiodo-2-methoxybenzene

溶剂

MTBE

反应条件

后处理

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

实验过程

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%).

来源