Methanol → 476199-03-8

HRID 1822961Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1822961
[F:1][C:2]1[C:10]2[S:9][C:8]([C:11]([O:13]C)=[O:12])=[CH:7][C:6]=2[C:5]([O:15][CH3:16])=[CH:4][CH:3]=1.[OH-].[Na+].CO>O>[F:1][C:2]1[C:10]2[S:9][C:8]([C:11]([OH:13])=[O:12])=[CH:7][C:6]=2[C:5]([O:15][CH3:16])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 22171205Methyl 7-fluoro-4-methoxy-1-benzothiophene-2-carboxylate

Produkt 1

HCID 23568964476199-03-8Ausbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A mixture of methyl 7-fluoro-4-methoxy-1-benzothiophene-2-carboxylate (67.2 g, 280 mmol), sodium hydroxide (45 g, 1.12 mol), methanol (800 mL) and water (400 mL) were stirred at ambient overnight. The methanol was evaporated and the mixture cooled to 0° C. Acidified with concentrated hydrochloric acid and stirred for 20 mins. The yellow solid was filtered, washing with water (3×100 mL). Dried under vacuum at 45° C. overnight, over phosphorus pentoxide to give the title compound (61.4 g, 97%); δH (300 MHz, d6-DMSO) 8.10 (1H, d, ArH) 7.44 (1H, t, ArH) 7.00 (1H, m, ArH) and 4.02 (3H, s, OCH3).

Aufarbeitung

  1. customThe methanol was evaporated
  2. stirringAcidified with concentrated hydrochloric acid and stirred for 20 mins
  3. filtrationThe yellow solid was filtered
  4. washwashing with water (3×100 mL)
  5. dry with materialDried under vacuum at 45° C. overnight, over phosphorus pentoxide

Quellen und Nachweise

ORD-Eintrag
ord-aaa46bb5ccac49cd935857785ed1c860
Quelldatensatz
uspto-grants-2006_05
Patentnummer
US07037932B2

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