Sulfuric Acid → p-Hydroxystyrene p-tert-butoxystyrene

HRID 1378897

反応式

HRID 1378897 の反応式
[CH:1]#[C:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.S(=O)(=O)(O)O>C(COC)OC>[C:3]([O:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:5]=1)([CH3:8])([CH3:4])[CH3:2].[OH:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]=[CH2:1])=[CH:4][CH:5]=1

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 327584-Ethynylphenol

生成物 1

HCID 68598693p-Hydroxystyrene p-tert-butoxystyrene

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of poly(p-hydroxystyrene) (4.0 g) [MARUKA LYNCUR-M, manufactured by Maruzen Petrochemical Co., Ltd., Mw 10000 and Mn 5000] in dimethoxyethane (70 ml) in a pressure vessel, isobutyrene (60 g) and conc. sulfuric acid (0.3 g) were added at -60° C. or lower. The mixture was brought to 45° C. for 1 hour with stirring, and then stirring was continued at room temperature for 22 hours. After reaction, the mixture was evaporated, and the residue was neutralized by sodium carbonate and poured into H2O. The precipitate was filtered by suction, washed was H2O and dried in vacuo to give 4.1 g of poly(p-tert-butoxystyrene/p-hydroxystyrene) as a white powder having Mw 10000 (GPC with polystyrene calibration). 1HNMR analysis indicated that 50% of p-hydroxy group was converted into p-tert-butoxy group.

後処理

  1. stirringstirring
  2. waitwas continued at room temperature for 22 hours
  3. customAfter reaction
  4. customthe mixture was evaporated
  5. additionpoured into H2O
  6. filtrationThe precipitate was filtered by suction
  7. washwashed
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-9fcb89fefbcb43e5a7b3f17879fc26ad
出典データセット
uspto-grants-1997_09
特許番号
US05670299

関連ノート

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