Water → HCID 57742154, Verbindung

HRID 660308Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 660308
[OH:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].Cl[CH2:17][O:18][CH3:19].O>C1COCC1>[CH3:17][O:18][CH2:19][O:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][CH:7]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 7864Chloromethyl Methyl EtherHCID 24758Sodium hydrideHCID 572437Ethyl (3-Hydroxyphenyl)acetate

Produkt 1

HCID 57742154HCID 57742154, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Ethyl 2-(3-hydroxyphenyl)acetate (24 g, 80.51 mmol) in THF (100 mL) was slowly added sodium hydride (2.93 g, 73.3 mmol) and chloromethylmethylether (5.94 g, 73.7 mmol) at 0° C. The reaction mixture was stirred for 16 hours at room temperature. The mixture was added water (200 mL) and extracted with EtOAc. The organic layer was dried with MgSO4. The organic layer was filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography eluting with n-Hexane/EtOAc=10/1.

Aufarbeitung

  1. customat 0° C
  2. extractionextracted with EtOAc
  3. dry with materialThe organic layer was dried with MgSO4
  4. filtrationThe organic layer was filtered
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe residue was purified by column chromatography
  7. washeluting with n-Hexane/EtOAc=10/1

Quellen und Nachweise

ORD-Eintrag
ord-21179bb2e1e7436489c4de8b8706901a
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08084484B2

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