反应 #2770

ord-5a412429988a4f6d803dc50ce52e1efd

反应方程式

O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
C1=COCCC1
3,4-dihydro-2H-pyran
O=S(=O)(O)O
sulfuric acid
C#Cc1ccc(O)cc1
Poly(p-hydroxystyrene)
C=Cc1ccc(O)cc1.C=Cc1ccc(OC2CCCCO2)cc1
p-tetrahydropyranyloxystyrene p-hydroxystyrene

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩the reaction solution was concentrated under reduced pressure
  2. 2
    其他The residue obtained
  3. 3
    其他to precipitate crystals
  4. 4
    过滤The crystals were filtered off
  5. 5
    洗涤washed with water
  6. 6
    其他dried under reduced pressure

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05731123uspto-grants-1998_03