Reaktion #1998554

ord-9df146c3a5e34ea7a1e3b0a1181fec57

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstige5-[(3,5-Dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine was prepared
  2. 2
    FiltrationThe reaction mixture was filtered
  3. 3
    WaschenMP carbonate was washed with 10% MeOH in DCM
  4. 4
    SonstigeThis was evaporated to dryness

Vorschrift

5-[(3,5-Dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine was prepared as follows: MP carbonate (2.74 mmol/g) (12.00 g, 32.88 mmol) was added to 5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine hydrochloride (5 g, 17.50 mmol) in methanol (200 mL) and water (20 mL). The resulting suspension was stirred at room temperature for 18 h. The reaction mixture was filtered and MP carbonate was washed with 10% MeOH in DCM. This was evaporated to dryness to afford 5-[(3,5-dimethoxyphenyl)methoxy]-2H-pyrazol-3-amine (2.94 g, 67.5%) as an orange waxy solid. 1H NMR (399.9 MHz, DMSO-d6) δ 3.74 (6H, s), 4.76 (1H, s), 4.97 (2H, s), 6.42 (1H, t), 6.55 (2H, d).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08604022B2uspto-grants-2013_12