반응 #626984

ord-1b9a8b9cbf8b41479662168055907838

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture is concentrated
  2. 2
    workup.ADDITIONwater is added
  3. 3
    농축The mixture is concentrated
  4. 4
    기타to form solid from aqueous solution
  5. 5
    온도The mixture is frozen
  6. 6
    기타water is removed on a lyophilizer

실험 절차

A 40-mL vial is charged with N-(2-methyl-5-(6-(3,4,5-trimethoxybenzylamino)imidazo[1,2-b]pyridazin-2-yl)phenyl)pivalamide (0.604 g, 1.2 mmol) and TFA (5 mL) and the mixture is stirred at 50° C. for 16 hours. The reaction mixture is concentrated, taken up in CH3CN and water is added. The mixture is concentrated to form solid from aqueous solution. The mixture is frozen and water is removed on a lyophilizer to afford the title compound (0.350 g). LCMS (m/z)=324.5 [M+H]+, tR=1.96 min.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08871767B2uspto-grants-2014_10