Tetrahydrofuran → HCID 86662689, Verbindung

HRID 1746335Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1746335
[C:1]1([CH2:17][CH2:18][CH2:19][CH2:20]O)[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(N(CC)CC)C.[C:29](Cl)(=[O:33])[C:30]([CH3:32])=[CH2:31].[O:35]1CCCC1>>[C:29]([O:33][CH:17]([C:1]1[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)[CH2:18][CH2:19][CH3:20])(=[O:35])[C:30]([CH3:32])=[CH2:31]

Komponenten

5

Edukt 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 27626721-Pyrenebutanol

Produkt 1

HCID 86662689HCID 86662689, Verbindung

Versuchsvorschrift

In 100 ml of tetrahydrofuran, 5.0 g of 1-pyrenebutanol and 3.68 g of triethylamine were dissolved, and 1.90 g of methacryloyl chloride was added dropwise thereto at 0° C., followed by stirring at room temperature for 1 hour. A deposited material was filtered while being washed with ethyl acetate. The filtrate and the washing liquid were mixed. After the mixture was dried with magnesium sulfate, the solvent was removed by evaporation under a reduced pressure. A residue was purified by a column chromatograph (silica gel, hexane:ethyl acetate=10:1), and vacuum-dried to thus obtain 1-pyrenylbutyl methacrylate.

Aufarbeitung

  1. customat 0° C.
  2. filtrationA deposited material was filtered
  3. washwhile being washed with ethyl acetate
  4. additionThe filtrate and the washing liquid were mixed
  5. dry with materialAfter the mixture was dried with magnesium sulfate
  6. customthe solvent was removed by evaporation under a reduced pressure
  7. customA residue was purified by a column chromatograph (silica gel, hexane:ethyl acetate=10:1)
  8. dry with materialvacuum-dried to thus obtain 1-pyrenylbutyl methacrylate

Quellen und Nachweise

ORD-Eintrag
ord-7416e88d2e8b466a9a4890b54f645be9
Quelldatensatz
uspto-grants-2015_10
Patentnummer
US09150414B2

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