Water → HCID 20138923, Verbindung

HRID 1905749Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1905749
[C:1]([CH:3]1[C:6]2=[CH:7][C:8]([O:11][CH3:12])=[CH:9][CH:10]=[C:5]2[CH2:4]1)#[N:2].[H-].[Na+].[CH3:15]I.O>C1COCC1.C(OCC)C>[C:1]([C:3]1([CH3:15])[C:6]2=[CH:7][C:8]([O:11][CH3:12])=[CH:9][CH:10]=[C:5]2[CH2:4]1)#[N:2]

Komponenten

7

Edukt 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 12238660Bicyclo[4.2.0]octa-1,3,5-triene-7-carbonitrile, 4-methoxy-

Produkt 1

HCID 20138923HCID 20138923, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 1-cyano-5-methoxybenzocyclobutene (47.3 ml) in THF (300 ml) is added dropwise to a stirred suspension of NaH (23.8 g, 60% in mineral oil) and methyl iodide (37 ml) in THF (300 ml) under nitrogen and the reaction mixture is stirred at RT for three hours. H2O is added to the reaction mixture which is diluted with diethyl ether, washed with water, 10% aq. sodium sulphite, sat'd sodium chloride, dried, filtered and the filtrate evaporated in vacuo affording the desired product as a yellow oil.

Aufarbeitung

  1. washwashed with water, 10% aq. sodium sulphite
  2. customdried
  3. filtrationfiltered
  4. customthe filtrate evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8e875d6d17e64a8fa8636ba93a67316d
Quelldatensatz
uspto-grants-1987_03
Patentnummer
US04647559

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