N-Methylethylenediamine → HCID 178509325, Verbindung

HRID 2097966Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2097966
[Br:1][C:2]1[C:6]2[C:7]3[N:8]([CH:11]=[N:12][N:13]=3)C=[N:10][C:5]=2[S:4][CH:3]=1.CNCCN>CO.[Cl-].[NH4+]>[Br:1][C:2]1[C:6]([C:7]2[NH:8][CH:11]=[N:12][N:13]=2)=[C:5]([NH2:10])[S:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 8014N-MethylethylenediamineHCID 596366779-Bromothieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

Produkt 1

HCID 178509325HCID 178509325, VerbindungAusbeute 99,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 25517Ammonium ChlorideLösungsmittel

Versuchsvorschrift

9-Bromothieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (551 mg, 2.16 mmol) and N-methylethane-1,2-diamine (1 ml, 11.3 mmol) in methanol (20 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 525 mg (99% yield) of 4-bromo-3-(4H-1,2,4-triazol-3-yl)thiophen-2-amine as a brown solid. Method [8] retention time 2.25 min by HPLC (M+245 and 247).

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-106778288eb14b6e81346b786b9bdff2
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08450363B2

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