Reaktion #2185226

Reaktionsgleichung

9-Chloro-3-methylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine

N-methylethane-1,2-diamine

→

4-chloro-3-(3-methyl-1H-1,2,4-triazol-5-yl)thiophen-2-amine

Ausbeute 88.1%

Lösungsmittel

ammonium chloride

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with methylene chloride
2. 2
   TrocknenThe combined organic extracts were dried over magnesium sulfate
3. 3
   Filtrationfiltered
4. 4
   Einengenconcentrated under reduced pressure

Vorschrift

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).

Quelle