Methyl iodide → HCID 13280935, Verbindung

HRID 1903630Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1903630
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[C:6]3[C:7](=[CH:18][NH:19][C:20]=3[CH3:21])[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.[CH3:24]C(C)([O-])C.[K+].CI>CN(C)C=O.O>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[C:6]3[C:7](=[CH:18][N:19]([CH3:24])[C:20]=3[CH3:21])[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1

Komponenten

6

Edukt 3

HCID 6328Methyl iodideHCID 13067111HCID 13067111, VerbindungHCID 23665647Potassium tert-butoxide

Produkt 1

HCID 13280935HCID 13280935, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

In one portion, 2.0 g (5.8) mmol) of 8-chloro-6-(2-chlorophenyl)-1-methyl-2H,4H-pyrrolo[3,4-d][2]benzazepine were added to an ice-cooled solution of 0.8 g (7.1 mmol) of potassium t-butoxide in 20 ml of dry dimethylformamide. After stirring at 0° C. for 10 minutes, 0.8 ml (12.8 mmol) of methyl iodide was added and the resulting solution was stirred for 20 minutes. The mixture was diluted with water, and the resulting precipitate was collected by filtration. The solid was dissolved in methylene chloride, dried over anhydrous sodium sulfate, and concentrated at reduced pressure to give 8-chloro-6-(2-chlorophenyl)-1,2-dimethyl-2H,4H-pyrrolo[3,4-d][2]benzazepine as orange prisms, mp 200°-202° C. A sample was recrystallized from a mixture of ether and methylene chloride to give pale yellow prisms, mp 203°-204° C.

Aufarbeitung

  1. stirringthe resulting solution was stirred for 20 minutes
  2. filtrationthe resulting precipitate was collected by filtration
  3. dissolutionThe solid was dissolved in methylene chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-29830dc37f8c4bac96ca648e2188f01b
Quelldatensatz
uspto-grants-1984_03
Patentnummer
US04436662

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