Vinyl Acetate → Vinyl 4-(pyren-1-yl)butanoate

HRID 2194326

반응식

HRID 2194326 반응식
[C:1]1([CH2:17][CH2:18][CH2:19][C:20]([OH:22])=[O:21])[C:14]2[C:15]3=[C:16]4[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][CH:8]=[C:7]4[CH:6]=[CH:5][C:4]3=[CH:3][CH:2]=1.[C:23](OC=C)(=O)[CH3:24]>C1(C)C=CC=CC=1>[C:1]1([CH2:17][CH2:18][CH2:19][C:20]([O:22][CH:23]=[CH2:24])=[O:21])[C:14]2[C:15]3=[C:16]4[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][CH:8]=[C:7]4[CH:6]=[CH:5][C:4]3=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 7904Vinyl Acetate2회HCID 769771-Pyrenebutanoic acid

생성물 1

HCID 86648107Vinyl 4-(pyren-1-yl)butanoate

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
60 °C

실험 절차

To a 500 mL, two neck flask equipped with a stir bar, argon inlet, and stopper is added 4-(1-Pyrenyl)butyric acid (10.0 grams, 34.7 mmol, obtained from Sigma-Aldrich, Milwaukee, Wis.), palladium acetate 1,10-phenanthroline complex (403 milligrams, 1 mmol) and vinyl acetate (128 milliliters, 1.39 mol, obtained from Sigma-Aldrich, Milwaukee, Wis.). Next, toluene (200 milliliters) is added, the solution is purged with argon and stirred magnetically at 60° C. for 62 hours. The excess vinyl acetate, along with acetic acid (co-product) is removed, an additional vinyl acetate (32 mL, 0.35 mol) is added, and the reaction is continued for 48 hours at 60° C. under argon to complete the reaction. The excess vinyl ester is removed, and the crude product is filtered to remove suspended catalyst residue, and the toluene is removed in vacuo to famish vinyl 4-(pyren-1-yl)butanoate.

후처리

  1. customTo a 500 mL, two neck flask equipped with a stir bar, argon inlet
  2. customthe solution is purged with argon
  3. customThe excess vinyl acetate, along with acetic acid (co-product) is removed
  4. waitthe reaction is continued for 48 hours at 60° C. under argon
  5. customthe reaction
  6. customThe excess vinyl ester is removed
  7. filtrationthe crude product is filtered
  8. customto remove
  9. customthe toluene is removed in vacuo to famish vinyl 4-(pyren-1-yl)butanoate

출처 및 근거

ORD 기록
ord-83c7edf7d9ca4a1985a106b167cd6f67
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08334026B2

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