Reaktion #1705907

ord-b6c3ea7cfc7d45f3904a0fcdf1b595b7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeevaporated in vacuo
  2. 2
    workup.DISSOLUTIONThe resulting residue was dissolved in DCM (40 mL)
  3. 3
    Waschenwashed with NaHCO3 (20 mL, saturated aqueous solution)
  4. 4
    TrocknenThe separated organic layer was dried over MgSO4
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigeevaporated in vacuo

Vorschrift

To a stirred solution of tert-butyl 7-morpholino-2,3-dihydro-1H-pyrido[2,3-b]-[1,4]thiazine-1-carboxylate (280 mg, 0.83 mmol) in DCM (2.0 mL) was added TFA (3.2 mL, 41.5 mmol). The reaction was stirred at rt for 2 h and evaporated in vacuo. The resulting residue was dissolved in DCM (40 mL) and washed with NaHCO3 (20 mL, saturated aqueous solution). The separated organic layer was dried over MgSO4, filtered and evaporated in vacuo to give 4-(2,3-dihydro-1H-pyrido[2,3-b][1,4]thiazin-7-yl)morpholine as a white solid. 1H NMR (400 MHz, chloroform-d) δ ppm 7.62 (1H, d, J=2.5 Hz), 6.26 (1H, d, J=2.5 Hz), 3.82-3.87 (4H, m), 3.59-3.63 (2H, m), 3.13-3.17 (2H, m), 3.06-3.10 (4H, m). Mass Spectrum (ESI) m/e=238.2 (M+1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08765940B2uspto-grants-2014_07