Sulfuric Acid → p-Hydroxystyrene p-tetrahydropyranyloxystyrene

HRID 2674

반응식

HRID 2674 반응식
[CH:1]#[C:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[O:10]1[CH:15]=[CH:14][CH2:13][CH2:12][CH2:11]1.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>C(COC)OC.O>[O:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]1[O:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:5]=1.[OH:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:5]=1

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 80803,4-dihydro-2H-pyranHCID 10340Sodium CarbonateHCID 327584-Ethynylphenol

생성물 1

HCID 67686066p-Hydroxystyrene p-tetrahydropyranyloxystyrene

시약·촉매·용매 2

HCID 962Water용매HCID 80711,2-Dimethoxyethane용매

실험 절차

Poly(p-hydroxystyrene) (weight average molecular weight: 9,600) in an amount of 9 g was dissolved in 100 ml of dimethoxyethane, and thereto 12.6 g of 3,4-dihydro-2H-pyran and 0.5 ml of sulfuric acid were added. This solution was stirred for 15 hours at 30°-40° C. After the reaction was completed, the reaction solution was concentrated under reduced pressure. The residue obtained was neutralized with sodium carbonate, and then poured into water to precipitate crystals. The crystals were filtered off, washed with water and dried under reduced pressure. Thus, 11.0 g of poly(p-tetrahydropyranyloxystyrene-p-hydroxystyrene) was obtained as white powder. The ratio of the p-tetrahydropyranyloxystyrene units to the p-hydroxystyrene units in the polymer obtained was determined to be 3:7 by 1H-NMR analysis.

후처리

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. customThe residue obtained
  3. customto precipitate crystals
  4. filtrationThe crystals were filtered off
  5. washwashed with water
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-5a412429988a4f6d803dc50ce52e1efd
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731123

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