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Methyl iodide → HCID 23372624, Verbindung

HRID 1862974
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1862974
[CH3:1][C:2]1[CH:3]=[C:4]([CH3:20])[C:5]2[C:11](=[O:12])[NH:10][C:9]3[CH:13]=[C:14]([CH3:18])[C:15]([CH3:17])=[CH:16][C:8]=3[NH:7][C:6]=2[N:19]=1.[H-].[Na+].[CH3:23]I>CN(C)C=O>[CH3:1][C:2]1[CH:3]=[C:4]([CH3:20])[C:5]2[C:11](=[O:12])[N:10]([CH3:23])[C:9]3[CH:13]=[C:14]([CH3:18])[C:15]([CH3:17])=[CH:16][C:8]=3[NH:7][C:6]=2[N:19]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 20393029HCID 20393029, Verbindung

Produkt 1

HCID 23372624HCID 23372624, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A mixture consisting of 6.7 gm of 6,11-dihydro-2,4,8,9-tetramethyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, 150 ml of dimethyl formamide and 1.4 gm of 50% sodium hydride in mineral oil was stirred at 50° C. in a nitrogen atmosphere for 30 minutes. Thereafter, a solution of 7.1 gm of methyl iodide in 30 ml of dimethyl formamide was added dropwise at room temperature. The resulting mixture was heated on an oil bath at 120° C. for 1 hour, and was then evaporated in vacuo. The residue was admixed with water, the aqueous mixture was made alkaline with ammonia, and it was then extracted with chloroform. After separation of the 2,4,6,8,9,11-hexamethyl compound which had simultaneously formed in a silica gel column, the product was recrystallized from petroleum ether (b.p. 100°-140° C.), yielding 63% of theory of the compound named in the heading, which had a melting point of 225°-227° C.

Aufarbeitung

  1. temperatureThe resulting mixture was heated on an oil bath at 120° C. for 1 hour
  2. customwas then evaporated in vacuo
  3. extractionwas then extracted with chloroform
  4. customAfter separation of the 2,4,6,8,9,11-hexamethyl compound which
  5. customhad simultaneously formed in a silica gel column
  6. customthe product was recrystallized from petroleum ether (b.p. 100°-140° C.)
  7. customyielding 63% of theory of the compound

Quellen und Nachweise

ORD-Eintrag
ord-8ce8c33497504101a415110f4d1d8d29
Quelldatensatz
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04167570

Notizen zur Reaktion

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