Reacción #218684

ord-09f59616d81c4d1e8bb8ee11eda3ff41

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroat ambient temperature
  2. 2
    Otropurification by flash chromatography
  3. 3
    Lavadoeluting with a gradient of a 5% solution of 2M ammonia in methanol, in dichloromethane

Procedimiento

Using the method of Example 346 using (5)-10-[3-(2-methoxy-ethyl)-piperazin-1-yl]-2-trifluoromethyl-4H-3-thia-1,4,9-triaza-benzo[f]azulene and acetaldehyde at ambient temperature, and purification by flash chromatography, eluting with a gradient of a 5% solution of 2M ammonia in methanol, in dichloromethane, (0-50% over 25 minutes, 50% for 10 minutes, 50-100% over 23 minutes, 100% for 5 minutes) gives the title compound: mass spectrum (APCI, m/e): 440 (M+1); NMR (1H, 300 MHz, DMSO-d6), δ (ppm): δ 8.47 (s, 1H), 6.96-6.81 (m, 3H), 6.71 (m, 1H), 3.50 (br. m, 3H), 3.35-3.21 (m, 2H), 3.21-3.07 (m, 4H), 2.76-2.51 (m, 3H), 2.37 (m, 2H), 1.67 (m, 2H), 0.96 (t, 3H, J=6.9 Hz).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07384934B2uspto-grants-2008_06