Reaktion #1607009

ord-b602bef976c04376bb9b5d91daca43e8

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

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-isopropylthieno[3,2-e][1,2,4]triazolo[4,3-c]pyrimidine (300 mg, 1.19 mmol) and N-methylethane-1,2-diamine (0.50 ml, 5.67 mmol) in methanol (10 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 yield 4-chloro-3-(3-isopropyl-1H-1,2,4-triazol-5-yl)thiophen-2-amine. Method [7] Retention time 1.39 min by HPLC (M+=243 and 245).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09073891B2uspto-grants-2015_07