反应 #1797483
ord-b8b43f53f80543279df9c954e3a0276b
反应方程式
反应物
试剂
反应条件
后处理
- 1其他a reactor similar to that of 1-1 was used
- 2workup.STIRRINGto stir a solution
- 3其他obtained
- 4其他obtained in 1-1
- 5温度by cooling in an ice water bath
- 6温度the solution was heated for 30 minutes at 40° C.
- 7其他was adjusted to 20° C.
- 8其他a solution obtained
- 9workup.STIRRINGwhile stirring
- 10温度the solution was heated to 40° C. for 30 minutes
实验过程
The monoisobutylphthalic acid obtained in 1-1 was formed into a triethylamine salt in anhydrous ethanol, after which an ethanol solution of neodymium nitrate was added while stirring. That is, a reactor similar to that of 1-1 was used to stir a solution obtained by adding 30 ml of an anhydrous ethanol to 70.0 g of the monoisobutylphthalic acid obtained in 1-1, while dripping 30.4 g of triethylamine while maintaining at 20° C. by cooling in an ice water bath. After dripping, the solution was heated for 30 minutes at 40° C. to prepare a synthesis solution of monoisobutylphthalic acid-triethylamine salts. Next, this synthesis solution was adjusted to 20° C., and a solution obtained by dissolving 43.8 g of neodymium nitrate into 100 ml of ethanol was dripped in while stirring. After dripping, the solution was heated to 40° C. for 30 minutes, to produce a synthesis solution of a neodymium salt of monoisobutylphthalic acid. Then, ethanol was distilled from this synthesis solution to concentrate, 150 ml of chloroform and 200 ml of water were added to the concentrate and stirred, and the resulting neodymium salt of monoisobutylphthalic acid was extracted and washed. After further washing this chloroform solution with water twice, it was transferred to a 2 L cylindrical separable flask, and 800 ml of hexane were slowly added while stirring to crystallize. Crystals obtained by filtering this slurry solution, then further the filtered crystals were added to 400 ml of hexane, stirred and washed, then refiltered, and the crystals were dried under reduced pressure at 50° C., to obtain 68.1 g of a neodymium salt of monoisobutylphthalic acid (yield 84%).