Propylene glycol methyl ether acetate → p-(1-(Cyclohexylethoxy)ethoxy)styrene p-Hydroxystyrene

HRID 353683

반응식

HRID 353683 반응식
[CH:1]#[C:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[C:10]([O:13][CH:14]([CH3:18])[CH2:15]OC)(=[O:12])[CH3:11]>>[CH:3]1([CH2:2][CH2:1][O:12][CH:10]([O:13][C:14]2[CH:15]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:18]=2)[CH3:11])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.[OH:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:5]=1

참가 물질

3

반응물 2

HCID 7946Propylene glycol methyl ether acetateHCID 327584-Ethynylphenol

생성물 1

HCID 86598586p-(1-(Cyclohexylethoxy)ethoxy)styrene p-Hydroxystyrene수율 69.3%

반응 조건

온도
20 °C

실험 절차

In 320 g of propylene glycol monomethyl ether acetate (PGMEA) was dissolved 70 g of poly(p-hydroxystyrene) (VP-8000, manufactured by Nippon Soda Co., Ltd.) with heating and the solution was subjected to dehydration by distillation under a reduce pressure and cooled to 20° C. To the solution were added 0.35 g of pyridinium p-toluenesulfonate and 22.4 g of 2-cyclohexylethanol. Then, 17.5 g of tert-butyl vinyl ether was gradually added to the solution, followed by reacting at 20° C. for 5 hours. To the reaction mixture were added 0.28 g of triethylamine and 320 ml of ethyl acetate and the mixture was washed three times with each 150 ml of distilled water. The solvent was distilled off to concentrate, the resulting oily substance was dissolved in 100 ml of acetone and the solution was gradually poured into 2 liters of distilled water. The powder thus-deposited was collected by filtration and dried to obtain 54 g of the desired compound. The Mw of the resin was 12,000 and the molecular weight distribution (Mw/Mn) thereof was 1.1.

후처리

  1. temperaturewith heating
  2. distillationthe solution was subjected to dehydration by distillation under a reduce pressure
  3. additionTo the solution were added 0.35 g of pyridinium p-toluenesulfonate and 22.4 g of 2-cyclohexylethanol
  4. additionThen, 17.5 g of tert-butyl vinyl ether was gradually added to the solution
  5. additionTo the reaction mixture were added 0.28 g of triethylamine and 320 ml of ethyl acetate
  6. washthe mixture was washed three times with each 150 ml of distilled water
  7. distillationThe solvent was distilled off
  8. concentrationto concentrate
  9. dissolutionthe resulting oily substance was dissolved in 100 ml of acetone
  10. additionthe solution was gradually poured into 2 liters of distilled water
  11. filtrationThe powder thus-deposited was collected by filtration
  12. customdried

출처 및 근거

ORD 기록
ord-c34343c0dabe40fc82375b76a7b8d25f
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756179B2

연결된 노트

불러오는 중…