N-Methylethylenediamine → HCID 178434595, Verbindung

HRID 1519831Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1519831
[Cl:1][C:2]1[C:6]2[C:7]3[N:8]([C:11]([CH3:14])=[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]([CH3:14])[N:8]=2)=[C:5]([NH2:10])[S:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 8014N-MethylethylenediamineHCID 687822379-Chloro-3-methylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

Produkt 1

HCID 178434595HCID 178434595, VerbindungAusbeute 88,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 25517Ammonium ChlorideLösungsmittel

Versuchsvorschrift

9-Chloro-3-methylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (82 mg, 365 umol) and N-methylethane-1,2-diamine (0.30 ml, 3.40 mmol) 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 69 mg (88% yield) of 4-chloro-3-(3-methyl-1H-1,2,4-triazol-5-yl)thiophen-2-amine as a yellow solid. Method [1] Retention time 0.61 min by HPLC (M+=215 and 217).

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-98e333faafda4ecf8aad85fea2556d14
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073891B2

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