N-Methylethylenediamine → HCID 178438043, Verbindung

HRID 1519829Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1519829
[Cl:1][C:2]1[C:6]2[C:7]3[N:8]([C:11]([CH2:14][CH3:15])=[N:12][N:13]=3)C=[N:10][C:5]=2[S:4][CH:3]=1.CNCCN>CO.[Cl-].[NH4+]>[Cl:1][C:2]1[C:6]([C:7]2[NH:13][N:12]=[C:11]([CH2:14][CH3:15])[N:8]=2)=[C:5]([NH2:10])[S:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 8014N-MethylethylenediamineHCID 687851919-Chloro-3-ethylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

Produkt 1

HCID 178438043HCID 178438043, VerbindungAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 25517Ammonium ChlorideLösungsmittel

Versuchsvorschrift

9-Chloro-3-ethylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (20 mg, 83.8 umol) and N-methylethane-1,2-diamine (0.05 ml, 5.67 umol) in methanol (2 ml) was placed into a preheated oil bath at 60° C. After stirring for 15 min, the solution was diluted with saturated ammonium chloride and extracted with methylene chloride. The combined organic extracts were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to afford 18 mg (94% yield) of 4-chloro-3-(3-ethyl-1H-1,2,4-triazol-5-yl)thiophen-2-amine as a brown solid. Method [8] Retention time 2.63 min by HPLC (M+ 229 and 231).

Aufarbeitung

  1. extractionextracted with methylene chloride
  2. dry with materialThe combined organic extracts were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b85cdb9a13ad435e850b385641caf734
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073891B2

Notizen zur Reaktion

Wird geladen…