반응 #1797485
ord-3f502ade04384591b6203b31e27cdd69
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후처리
- 1기타a reactor similar to the above was used
- 2workup.STIRRINGto stir a solution
- 3기타obtained
- 4기타obtained in 5-1
- 5온도while maintaining at 30° C. or less
- 6온도by cooling in an ice water bath
- 7기타was adjusted to 20° C.
- 8기타a solution obtained
- 9workup.STIRRINGwhile stirring
- 10온도the solution was heated to 40° C. for 30 minutes
실험 절차
The mono-n-butylphthalic acid obtained in 5-1 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 the above was used to stir a solution obtained by adding 30 ml of an anhydrous ethanol to 68.1 g of the mono-n-butylphthalic acid obtained in 5-1, while dripping 30.4 g of triethylamine while maintaining at 30° C. or less 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 mono-n-butylphthalic acid-triethylamine salt. 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 mono-n-butylphthalic 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 mono-n-butylphthalic acid was extracted and washed. After further washing this chloroform solution with, water twice, the chloroform was distilled out. The solid obtained by distillation was crushed, then dried under reduced pressure at 50° C. to obtain 72.9 g of a neodymium salt of mono-n-butylphthalic acid (yield 90%).