Sulfuric Acid → p-Hydroxystyrene p-tetrahydropyranyloxystyrene

HRID 2674

反応式

HRID 2674 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 67686066p-Hydroxystyrene p-tetrahydropyranyloxystyrene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5a412429988a4f6d803dc50ce52e1efd
出典データセット
uspto-grants-1998_03
特許番号
US05731123

関連ノート

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