تفاعل #1114528

معادلة التفاعل

potassium carbonate

poly(p-hydroxystyrene)

ethyl acetate

ethyl acetate

→

PGMEA

المذيبات

acetic acid

dimethylsulfoxide

—

ice water

water

water

ظروف التفاعل

المعالجة

1. 1
   أخرىwas returned to room temperature
2. 2
   workup.ADDITIONby little added to the reaction solution
3. 3
   أخرىThe reaction solution was transferred to a separating funnel
4. 4
   workup.STIRRINGAfter stirring
5. 5
   أخرىthe aqueous layer was removed
6. 6
   غسيلthe organic layer was washed with 200 mL of distilled water five times
7. 7
   تركيزThe organic layer was then concentrated
8. 8
   workup.DISSOLUTIONdissolved in 120 g of tetrahydrofuran (THF)
9. 9
   workup.ADDITIONThereto, 26.53 g of triethylamine was added
10. 10
    درجة الحرارةthe reaction solution was cooled to 0° C
11. 11
    workup.ADDITIONFurthermore, 23.43 g of the 3-chloro-3-benzyloxypropionitrile solution above was added dropwise
12. 12
    أخرىwas returned to room temperature
13. 13
    workup.STIRRINGstirred for 4 hours
14. 14
    workup.ADDITIONAfter adding 200 ml of distilled water to the reaction solution, THF
15. 15
    أخرىwas removed by an evaporator, and 200 mL of ethyl acetate
16. 16
    workup.ADDITIONwas added to the residue
17. 17
    أخرىThe reaction solution was transferred to a separating funnel
18. 18
    أخرىthe aqueous layer was removed
19. 19
    غسيلThe organic layer was washed with 200 ml of distilled water three times
20. 20
    تركيزconcentrated to about 150 mL by an evaporator
21. 21
    workup.ADDITIONadded dropwise in 2 L of hexane
22. 22
    workup.ALIQUOTA part of the obtained precipitate was sampled for NMR measurement
23. 23
    workup.DISSOLUTIONthe remaining was dissolved in 75 g of PGMEA
24. 24
    أخرىFrom the obtained solution, the low boiling point solvent was removed by an evaporator

الإجراء التجريبي

30 g of poly(p-hydroxystyrene) (VP8000) produced by Nippon Soda Co., Ltd. was dissolved in 120 mL of dimethylsulfoxide (DMSO), and 2.21 g of 1-chloromethylnaphthalene, 34.51 g of potassium carbonate and 0.56 g of sodium iodide were added thereto. The mixture was stirred at 70° C. for 4 hours, and the reaction solution was returned to room temperature. Thereafter, 100 mL of ethyl acetate and 100 mL of distilled water were added thereto, and 130 g of an aqueous 23% acetic acid solution was little by little added to the reaction solution while stirring the reaction solution in ice water. The reaction solution was transferred to a separating funnel, and 100 mL of ethyl acetate and 100 mL of distilled water were further added. After stirring, the aqueous layer was removed, and the organic layer was washed with 200 mL of distilled water five times. The organic layer was then concentrated and dissolved in 120 g of tetrahydrofuran (THF). Thereto, 26.53 g of triethylamine was added, and the reaction solution was cooled to 0° C. Furthermore, 23.43 g of the 3-chloro-3-benzyloxypropionitrile solution above was added dropwise, and the reaction solution was returned to room temperature and then stirred for 4 hours. After adding 200 ml of distilled water to the reaction solution, THF was removed by an evaporator, and 200 mL of ethyl acetate was added to the residue. The reaction solution was transferred to a separating funnel, and the aqueous layer was removed. The organic layer was washed with 200 ml of distilled water three times, concentrated to about 150 mL by an evaporator and added dropwise in 2 L of hexane. A part of the obtained precipitate was sampled for NMR measurement, and the remaining was dissolved in 75 g of PGMEA. From the obtained solution, the low boiling point solvent was removed by an evaporator to obtain 105.2 g of a PGMEA solution (29.6 mass %) of Resin (P-22).

المصدر