반응 #1797488
ord-f3aaec8856f24ac2b20a52a986e169b1
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후처리
- 1기타Specifically, a reactor similar to that of 1-1 was used
- 2workup.STIRRINGto stir a solution
- 3기타obtained
- 4온도by cooling in an ice water bath
- 5온도the solution was heated for 30 minutes at 40° C.
- 6온도Next, this synthesis solution was maintained at about 30° C.
- 7기타a solution obtained
- 8workup.STIRRINGwhile stirring
- 9온도the clouding increased with time
- 10기타30 minutes
- 11온도the solution was heated to 40° C. for 30 minutes
실험 절차
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%).