Reaktion #333855

ord-1581bc42fc2b4cf18adf71249009b114

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated to 80 degree overnight
  2. 2
    Extraktionproduct extracted with dichloromethane (3×50 mL)
  3. 3
    Trocknencombined organics were dried with sodium sulfate
  4. 4
    Einengenconcentrated

Vorschrift

A mixture of 3-iodo-6-methyl-1H-indazole (516 mg, 2 mmol), 2-chloro-N,N-dimethylethanamine hydrochloride (346 mg, 2.4 mmol) and potassium carbonate (828 mg, 6 mmol) in 20 mL of DMF was heated to 80 degree overnight. After cooling to room temperature, water (50 mL) was added, product extracted with dichloromethane (3×50 mL), combined organics were dried with sodium sulfate, and concentrated to give 2-(3-iodo-6-methyl-1H-indazol-1-yl)-N,N-dimethylethanamine (1 g, 100%). 1H NMR (300 MHz, CDCl3): δ 7.33 (d, 1H, J=8.1 Hz), 7.15 (s, 1H), 7.03 (d, 1H, J=0.6 Hz), 4.47 (t, 2H, J=7.2 Hz), 2.81 (t, 2H, J=7.2 Hz), 2.51 (s, 3H), 2.34 (m, 6H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08658646B2uspto-grants-2014_02