Acetic Acid → p-Hydroxystyrene p-tert-butoxystyrene

HRID 1600506

反応式

HRID 1600506 の反応式
C([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH2:10])=[CH:7][CH:6]=1)(=O)C.[C:13]([O:17][C:18]1[CH:25]=[CH:24][C:21]([CH:22]=[CH2:23])=[CH:20][CH:19]=1)([CH3:16])([CH3:15])[CH3:14].[OH-].C[N+](C)(C)C.C(O)(=O)C>C(O)(C)C>[OH:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH2:10])=[CH:7][CH:6]=1.[C:13]([O:17][C:18]1[CH:19]=[CH:20][C:21]([CH:22]=[CH2:23])=[CH:24][CH:25]=1)([CH3:16])([CH3:14])[CH3:15]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 60966Tetramethylammonium hydroxideHCID 86754729p-Acetyloxystyrene p-tert-butoxystyrene

生成物 1

HCID 68598693p-Hydroxystyrene p-tert-butoxystyrene

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 46.3 g of poly(p-acetyloxystyrene/p-tert-butoxystyrene) obtained according to (1) above and 100 ml of a 16% aqueous solution of tetramethylammonium hydroxide was refluxed with stirring in 300 ml of isopropanol for 4 hours. The reaction solution was neutralized with acetic acid and concentrated under reduced pressure, and the residue was dissolved in 150 ml of acetone and poured into 5,000 ml of water to cause crystallization. Precipitated crystals were filtered out, washed with water and dried in vacuo to give 33.8 g of poly(p-hydroxystyrene/p-tert-butoxystyrene). P-hydroxystyrene unit/p-tert-butoxystyrene unit molar ratio in the polymer≈3:1 (1HNMR). Mw≈8,540; Mw/Mn=1.30 (GPC with polystyrene calibration).

後処理

  1. customobtained
  2. temperaturewas refluxed
  3. concentrationconcentrated under reduced pressure
  4. dissolutionthe residue was dissolved in 150 ml of acetone
  5. additionpoured into 5,000 ml of water
  6. customcrystallization
  7. customPrecipitated crystals
  8. filtrationwere filtered out
  9. washwashed with water
  10. customdried in vacuo

出典と根拠

ORDレコード
ord-7a2e5da259204190be7fc49dc0104e2a
出典データセット
uspto-grants-1999_11
特許番号
US05976759

関連ノート

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