Réaction #1797487
ord-2a6000f4362f469faa5f484971395794
Équation de réaction
Réactifs
Réactifs
Conditions de réaction
Traitement
- 1Autrea reactor similar to the above was used
- 2workup.STIRRINGto stir a solution
- 3Autreobtained
- 4Autreobtained in 6-1
- 5Températurewhile maintaining at 30° C. or less
- 6Températureby cooling in an ice water bath
- 7Autrewas adjusted to 20° C.
- 8Autrea solution obtained
- 9workup.DISSOLUTIONby dissolving
- 10workup.STIRRINGwhile stirring
- 11Températurethe solution was heated to 40° C. for 2 hours
Mode opératoire
The mono(2-phenoxyethyl)phthalic acid obtained in 6-1 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 88.6 g of the mono(2-phenoxyethyl)phthalic acid obtained in 6-1, 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(2-phenoxyethyl)phthalic 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 2 hours, to produce a synthesis solution of a neodymium salt of mono(2-phenoxyethyl)phthalic acid. Then, ethanol was distilled from this synthesis solution to concentrate, 300 ml of dichloromethane were added to the concentrate to form a solution, this solution was transferred to a 1 L separating funnel, shaken after pouring 400 ml of water into this separating funnel, and the resulting neodymium salts of mono(2-phenoxyethyl)phthalic acid were washed. After further washing this dichloromethane solution twice with 400 ml of water, the dichloromethane was distilled out. The solid obtained by distillation was crushed, then dried under reduced pressure at 50° C. to obtain 94.0 g of a neodymium salt of mono(2-phenoxyethyl)phthalic acid (yield 94%).