반응 #1607009

ord-b602bef976c04376bb9b5d91daca43e8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with methylene chloride
  2. 2
    건조The combined organic extracts were dried over magnesium sulfate
  3. 3
    여과filtered
  4. 4
    농축concentrated under reduced pressure

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09073891B2uspto-grants-2015_07