Methanol → HCID 57826680, Verbindung

HRID 1845493Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1845493
[Br:1][C:2]1[CH:3]=[C:4]([C:10]([OH:12])=[O:11])[S:5][C:6]=1[CH2:7][CH2:8][CH3:9].S(=O)(=O)(O)O.O.[CH3:19]O>>[Br:1][C:2]1[CH:3]=[C:4]([C:10]([O:12][CH3:19])=[O:11])[S:5][C:6]=1[CH2:7][CH2:8][CH3:9]

Komponenten

5

Edukt 4

HCID 887MethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 38431344-bromo-5-propylthiophene-2-carboxylic acid

Produkt 1

HCID 57826680HCID 57826680, Verbindung

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of 4-bromo-5-propyl-2-thiophenecarboxylic acid (5.0 g, 20.07 mmol) in methanol (100 ml) was added sulfuric acid (5.35 ml, 100 mmol). The resulting solution stirred at 50° C. for 36 h. H2O (50 mL) was added the aqueous phase was washed several times with DCM. The combined organic fractions were washed with saturated NaHCO3, dried over Na2SO4, concentrated and used directly without further purification providing methyl 4-bromo-5-propyl-2-thiophenecarboxylate (5.1 g, 18.61 mmol, 93° A yield) as a yellow oil: LCMS (ES) m/e 262, 264 (M, M+2)+.

Aufarbeitung

  1. washwas washed several times with DCM
  2. washThe combined organic fractions were washed with saturated NaHCO3
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customused directly without further purification

Quellen und Nachweise

ORD-Eintrag
ord-898717dc3f2447ef809c968762099baf
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08946278B2

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