Acetic Acid → p-Hydroxystyrene p-tert-butoxystyrene

HRID 1600506

반응식

HRID 1600506 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 68598693p-Hydroxystyrene p-tert-butoxystyrene

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7a2e5da259204190be7fc49dc0104e2a
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05976759

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