2-(1-Benzo[b]thiophen-2-yl-1-methylethyl)-4-methoxy-benzoic acid → HCID 66835213, Verbindung

HRID 61866Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 61866
[S:1]1[C:5]([C:6]([C:9]2[CH:17]=[C:16]([O:18][CH3:19])[CH:15]=[CH:14][C:10]=2[C:11]([OH:13])=O)([CH3:8])[CH3:7])=[CH:4][C:3]2[CH:20]=[CH:21][CH:22]=[CH:23][C:2]1=2>O>[CH3:19][O:18][C:16]1[CH:17]=[C:9]2[C:10](=[CH:14][CH:15]=1)[C:11](=[O:13])[C:4]1[C:3]3[CH:20]=[CH:21][CH:22]=[CH:23][C:2]=3[S:1][C:5]=1[C:6]2([CH3:7])[CH3:8]

Komponenten

3

Edukt 1

HCID 668347002-(1-Benzo[b]thiophen-2-yl-1-methylethyl)-4-methoxy-benzoic acid

Produkt 1

HCID 66835213HCID 66835213, VerbindungAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To 2-(1-benzo[b]thiophen-2-yl-1-methylethyl)-4-methoxy-benzoic acid (Compound Z4, 68 mg, 0.22 mmol), polyphosphoric acid (3.5 g) was added, and the mixture was stirred for 1 hr at 100° C. under heating. The mixture was added with water, extracted with ethyl acetate and washed with water. The organic layer was dried over magnesium sulfate. The residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (41 mg, 63%).

Aufarbeitung

  1. temperatureunder heating
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customThe residues obtained
  6. concentrationafter concentration under reduced pressure
  7. customwere purified by silica gel column chromatography (ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-6bbfad9e6b2844568b529556b7db471e
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09440922B2

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