反応 #1797490

反応方程式

neodymium nitrate

triethylamine

triethylamine

neodymium nitrate

2-methoxybenzoic acid

→

neodymium

2-methoxybenzoic acid

収率 85.0%

溶媒

ethanol

ethanol

ethanol

ethanol

反応条件

後処理

1. 1
   その他Specifically, a reactor similar to that of 1-1 was used
2. 2
   workup.STIRRINGto stir a slurry solution
3. 3
   その他obtained
4. 4
   温度by cooling in an ice water bath
5. 5
   温度the solution was heated for 30 minutes at 40° C.
6. 6
   workup.STIRRINGNext, while stirring this synthesis solution
7. 7
   その他holding at 25° C.
8. 8
   その他a solution obtained
9. 9
   温度the solution was heated to 40° C.
10. 10
    温度the clouding increased with time
11. 11
    workup.WAITAfter another 20 minutes
12. 12
    workup.ADDITIONwere further added
13. 13
    workup.STIRRINGthe solution was stirred for another hour at 40° C.
14. 14
    温度cooled
15. 15
    その他the reaction
16. 16
    その他Next, crystals obtained
17. 17
    ろ過by filtering this slurry solution
18. 18
    workup.ADDITIONwere added to 200 ml of methanol
19. 19
    workup.STIRRINGstirred
20. 20
    洗浄washed
21. 21
    workup.ADDITION200 ml of methanol were once again added to the crystals
22. 22
    workup.STIRRINGstirred
23. 23
    洗浄washed
24. 24
    ろ過filtered
25. 25
    その他The resulting crystals were dried under reduced pressure at 50° C.

実験手順

The compound was synthesized by the same method as that for Synthesis Example 1-2 above, that is, after forming a triethylamine salt of 2-methoxybenzoic acid in anhydrous ethanol, an ethanol solution of neodymium nitrate was added while stirring. Specifically, a reactor similar to that of 1-1 was used to stir a slurry solution obtained by adding 100 ml of an anhydrous ethanol to 45.65 g (0.3 mol) of 2-methoxybenzoic acid, while dripping 30.4 g (0.3 mol) of triethylamine while maintaining at 20-30° C. by cooling in an ice water bath. After dripping about one-third of the triethylamine, the slurry disappeared and became transparent. After dripping, the solution was heated for 30 minutes at 40° C. to prepare a transparent synthesis solution of 2-methoxybenzoic acid-triethylamine salts. Next, while stirring this synthesis solution and holding at 25° C., a solution obtained by dissolving 43.8 g of neodymium nitrate into 120 ml of ethanol was dripped in. Upon completion of dripping, the solution was heated to 40° C., began to cloud after 40 minutes, and the clouding increased with time. After another 20 minutes, it became an extremely thick slurry solution, so 100 ml of ethanol were further added, and the solution was stirred for another hour at 40° C., then cooled to end the reaction. Next, 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 50.83 g of a neodymium salt of 2-methoxybenzoic acid (yield 85%).

出典