Reaktion #659464

ord-e3e68e3e9c52418e91095d2f86afdc64

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was evaporated to a solid
  2. 2
    Sonstigetriturated
  3. 3
    Filtrationfiltered with the aid of water
  4. 4
    Waschenwashed with a 1 N aqueous hydrochloric acid solution
  5. 5
    Sonstigedried

Vorschrift

Prepared from 5-(4-Methyl-5-trifluoromethyl-isoxazol-3-yl)-thiophene-2-carboxylic acid and 4-methoxypiperidine by the method described in Example 2 Method B. The reaction mixture was evaporated to a solid, triturated and filtered with the aid of water, then washed with a 1 N aqueous hydrochloric acid solution followed by water. The solid was air dried to afford product as a colorless solid (151 mg, 81%). 1H NMR (CDCl3) 1.64-1.72 (m, 2H), 1.86-1.93 (m, 2H), 2.33 (d, J=1.3, 3H), 3.36 (s, 3H), 3.47-3.58 (m, 3H), 3.87-3.95 (m, 2H), 7.29 (d, J=3.5, 1H), 7.42 (d, J=4.0, 1H). 13C NMR 7.9, 30.9, 42 (br), 56.1, 75.2, 114.7, 118.7 (q, J=271), 128.0, 129.1, 131.1, 140.3, 155.2 (q, J=40), 158.0, 162.7. 19F NMR −63.2. LC/MS 6.31 min, [M+1]+ 375.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09029397B2uspto-grants-2015_05