Triethylamine → Neodymium

Participants

Reaction Conditions

Reaction Steps

The mono(2-butoxyethyl)phthalic acid obtained in 10-1 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 50 ml of an anhydrous ethanol to 79.9 g of the mono(2-butoxyethyl)phthalic acid obtained in 10-1, while dripping 30.4 g of triethylamine while maintaining at 25° C. or less by cooling in an ice water bath. After dripping, the solution was heated for 1 hour at 40° C. to prepare a synthesis solution of mono(2-butoxyethyl)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 120 ml of ethanol was dripped in while stirring. After dripping, the solution was heated to 40° C. for 1 hour, to produce a synthesis solution of a neodymium salt of mono(2-butoxyethyl)phthalic acid. Then, ethanol was distilled from this synthesis solution to concentrate, 200 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-butoxyethyl)phthalic acid were washed. After further washing this chloromethane 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 78.1 g of a neodymium salt of mono(2-butoxyethyl)phthalic acid (yield 83%).

Provenance & Evidence