Reaktion #87589

ord-e4b9e1e9d5fd4d3da722fc2032d8c45a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeExcess of solvent was removed at low temperature
  2. 2
    SonstigeThe reaction mass was quenched in ice
  3. 3
    Filtrationfilter off

Vorschrift

To a solution of tert-butyl 2-(2,6-dichlorophenyl)-2-((3-methoxy-4-nitrobenzoyl) carbamoyl)hydrazinecarboxylate (1.0 g, 2.002 mmol) in DCM (20 mL) was added trifluoro acetic acid (2.0 mL). The reaction mass was stirred at RT for 2-3 h. Excess of solvent was removed at low temperature. The reaction mass was quenched in ice and filter off to afford 0.200 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 3.98 (s, 3H), 7.56-7.62 (m, 2H), 7.69-7.75 (m, 3H), 8.02 (d, J=8.4 Hz, 1H), 11-12 (br s, 1H); MS (m/z): 382.07 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09439890B2uspto-grants-2016_09