반응 #1056872

ord-349fddccf84648ff950a38a4b7c20c2b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was submitted to microwave irradiation (80° C., 30 min)
  2. 2
    여과the resultant precipitate was filtered
  3. 3
    기타dried
  4. 4
    기타The crude material was purified with flash chromatography (SiO2, 50% EtOAc/hexane)
  5. 5
    기타to afford a white solid

실험 절차

A mixture of the lithium salt of 2-(quinazolin-6-ylamino)-benzoic acid (Step B, 533 mg, 0.72 mmol), 4,4-dimethyl-1,2,3,4-tetrahydro-quinolin-7-ylamine (127 mg, 0.72 mmol), TBTU (462 mg, 1.44 mmol) and DIEA (0.25 mL, 1.44 mmol) in 3 mL of DMF was submitted to microwave irradiation (80° C., 30 min). Water (5 mL) was added to the mixture, and the resultant precipitate was filtered and dried. The crude material was purified with flash chromatography (SiO2, 50% EtOAc/hexane) to afford a white solid. MS (ES+): 424.0 (M+H)+. Calc'd for C26H25N5O: 423.51.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07307088B2uspto-grants-2007_12