Dimethyl Sulfate → HCID 18986212, Verbindung

HRID 2396825Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2396825
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([F:13])=[CH:10][CH:11]=2)[C:6](=[O:14])[CH2:5]1)(=[O:3])[CH3:2].[OH-].[Na+].S(OC)(O[CH3:21])(=O)=O>C(=O)(O)[O-].[Na+]>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([F:13])=[CH:10][CH:11]=2)[C:6]([O:14][CH3:21])=[CH:5]1)(=[O:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 189863261-Acetyl-5-fluoro-1,2-dihydro-3H-indol-3-one

Produkt 1

HCID 18986212HCID 18986212, VerbindungAusbeute 86 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 516892Sodium BicarbonateLösungsmittel

Versuchsvorschrift

A mixture of 1.6 g of 1-acetyl-5-fluoroindolin-3-one, 1.9 g of powdered sodium hydroxide and 28 ml of dimethyl sulfate was stirred at room temperature for two hours. After the addition of 240 ml of saturated sodium bicarbonate solution the mixture was stirred overnight and subsequently filtered. The residue was taken up in 100 ml of ether and 100 ml of ethyl acetate. The solution was dried over sodium sulfate, filtered and evaporated. There were obtained 1.47 g (86%) of 1-acetyl-5-fluoro-3-methoxyindole as greenish crystals with m.p. 124°-125°.

Aufarbeitung

  1. stirringwas stirred overnight
  2. filtrationsubsequently filtered
  3. dry with materialThe solution was dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-d458808d652b46499f344d6e802f1ed4
Quelldatensatz
uspto-grants-1996_02
Patentnummer
US05494928

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