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Hydrochloric Acid → 2-(1,2,3,4-Tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethanol

HRID 2268492
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2268492
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:10][CH2:11][CH2:12][CH:13]1[CH2:19][CH2:18][C:17]2[C:20]([O:30][CH3:31])=[C:21]([O:28][CH3:29])[C:22]([O:26][CH3:27])=[C:23]([O:24][CH3:25])[C:16]=2[CH2:15][CH2:14]1)(=O)C.Cl>C(OCC)C.O>[CH3:25][O:24][C:23]1[C:16]2[CH2:15][CH2:14][CH:13]([CH2:12][CH2:11][OH:10])[CH2:19][CH2:18][C:17]=2[C:20]([O:30][CH3:31])=[C:21]([O:28][CH3:29])[C:22]=1[O:26][CH3:27]
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Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 183485472-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethyl acetateHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 183486172-(1,2,3,4-Tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethanolAusbeute 98,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

To a suspension of lithium aluminum hydride (486 mg) in diethyl ether (20 ml) was dropwise added a solution of 2-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethyl acetate (3.00 g) in diethyl ether (10 ml) with cooling with ice. After the reaction mixture stirred for 30 min, 10% hydrochloric acid was added to the reaction mixture, which was diluted with water and extracted with ethyl acetate. The organic layer was washed with water, saturated aqueous sodium bicarbonate, water, and saturated aqueous sodium chloride, and dried. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography (hexane to hexane:ethyl acetate=1:1) to yield the entitled compound (2.60 g) as crystals.

Aufarbeitung

  1. temperaturewith cooling with ice
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water, saturated aqueous sodium bicarbonate, water, and saturated aqueous sodium chloride
  4. customdried
  5. customThe solvent was removed in vacuo
  6. customThe residue was purified by silica gel column chromatography (hexane to hexane:ethyl acetate=1:1)

Quellen und Nachweise

ORD-Eintrag
ord-2861c39f953b44c680112f31fae24301
Quelldatensatz
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06326369B1

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