反应 #1665339

反应方程式

antimony pentachloride

tributylphosphate

→

Antimony Pentachloride Butyl Phosphate

溶剂

methylene chloride

methylene chloride

methylene chloride

反应条件

后处理

1. 1
   workup.ADDITIONTo this yellow solution was added dropwise
2. 2
   workup.ADDITIONThe addition
3. 3
   温度cooling should not
4. 4
   workup.ADDITIONBy the end of the addition
5. 5
   其他after which time the solvent was removed by evaporation at reduced pressure
6. 6
   其他The dark brown liquid was thoroughly dried in vacuo (0.1 mm Hg)

实验过程

In a round bottom flask under a nitrogen atmosphere, 8.01 g (0.0268 M) of antimony pentachloride was dissolved in 100 ml of methylene chloride. To this yellow solution was added dropwise with stirring a solution of 7.13 g (0.0268 M) of tributylphosphate in 20 ml of methylene chloride. The addition was accomplished at a rate such that the exotherm did not become excessive, the temperature being kept below the reflux temperature of methylene chloride (cooling should not be required). By the end of the addition, the initial yellow color had changed to a light brown. The reaction mixture was stirred at ambient temperature for one hour, after which time the solvent was removed by evaporation at reduced pressure. The dark brown liquid was thoroughly dried in vacuo (0.1 mm Hg). NMR (CDCl3, TMS) δ4.45(9H,q,J=6.0 Hz), 1.85(6H,m), 1.50(6H,m), 1.00(6H,t,J=6.7 Hz).

来源