反应 #1797488

反应方程式

neodymium nitrate

neodymium nitrate

triethylamine

neodymium nitrate

phenoxyacetic acid

→

phenoxyacetic acid

neodymium

溶剂

methanol

methanol

methanol

反应条件

后处理

1. 1
   其他Specifically, a reactor similar to that of 1-1 was used
2. 2
   workup.STIRRINGto stir a solution
3. 3
   其他obtained
4. 4
   温度by cooling in an ice water bath
5. 5
   温度the solution was heated for 30 minutes at 40° C.
6. 6
   温度Next, this synthesis solution was maintained at about 30° C.
7. 7
   其他a solution obtained
8. 8
   workup.STIRRINGwhile stirring
9. 9
   温度the clouding increased with time
10. 10
    其他30 minutes
11. 11
    温度the solution was heated to 40° C. for 30 minutes

实验过程

The compound was synthesized by the same method as that for Synthesis Example 1-2 above, that is, after forming a triethylamine salt of phenoxyacetic acid in anhydrous methanol, a methanol solution of neodymium nitrate was added while stirring. Specifically, a reactor similar to that of 1-1 was used to stir a solution obtained by adding 100 ml of an anhydrous methanol to 45.65 g (0.3 mol) of phenoxyacetic acid, while dripping 30.4 g (0.3 mol) of triethylamine while maintaining at 25° C. by cooling in an ice water bath. After dripping, the solution was heated for 30 minutes at 40° C. to prepare a transparent synthesis solution of phenoxyacetic acid-triethylamine salts. Next, this synthesis solution was maintained at about 30° C., and a solution obtained by dissolving 43.8 g of neodymium nitrate into 100 ml of methanol was dripped in while stirring. Upon completion of the dripping of the neodymium nitrate solution, it began to cloud, and the clouding increased with time. 30 minutes after completion of dripping, the solution was heated to 40° C. for 30 minutes, to produce a slurry solution of a neodymium salt of phenoxyacetic acid. Crystals obtained by filtering this slurry solution were added to 200 ml of methanol, stirred and washed, then refiltered, and 200 ml of methanol were once again added to the crystals, stirred and washed, then filtered. The resulting crystals were dried under reduced pressure at 50° C., to obtain 38.8 g of a neodymium salt of phenoxyacetic acid (yield 65%).

来源