Reaktion #1114526

Reaktionsgleichung

poly(p-hydroxystyrene)

ethyl acetate

ethyl acetate

potassium carbonate

→

PGMEA

Lösungsmittel

acetic acid

water

water

dimethylsulfoxide

—

ice water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas returned to room temperature
2. 2
   workup.ADDITIONby little added to the reaction solution
3. 3
   SonstigeThe reaction solution was transferred to a separating funnel
4. 4
   workup.STIRRINGAfter stirring
5. 5
   Sonstigethe aqueous layer was removed
6. 6
   Waschenthe organic layer was washed with 200 mL of distilled water five times
7. 7
   EinengenThe organic layer was then concentrated to about 150 mL
8. 8
   workup.ADDITIONadded dropwise in 2 L of hexane
9. 9
   workup.ALIQUOTA part of the obtained precipitate was sampled for NMR measurement
10. 10
    workup.DISSOLUTIONthe remaining was dissolved in 70 g of PGMEA
11. 11
    SonstigeFrom the obtained solution, the low boiling point solvent was removed by an evaporator

Vorschrift

30 g of poly(p-hydroxystyrene) (VP8000) produced by Nippon Soda Co., Ltd. was dissolved in 120 mL of dimethylsulfoxide (DMSO), and 9.36 g of (1-ethyl)cyclopentyl bromoacetate, 9.70 g of Compound (p-9) above, 34.51 g of potassium carbonate and 0.89 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 mass % 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 to about 150 mL 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 70 g of PGMEA. From the obtained solution, the low boiling point solvent was removed by an evaporator to obtain 102.1 g of a PGMEA solution (34.6 mass %) of Resin (P-9).

Quelle