반응 #708948

ord-d3868f5a9bb8497fb7679dcfde3775f2

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타reacted at room temperature for 1 hour
  2. 2
    기타reacted overnight at room temperature
  3. 3
    기타The reaction mixture is evaporated under reduced pressure
  4. 4
    기타dried in vacuo
  5. 5
    기타the desired product purified by silica gel chromatography in the system CH2Cl2 :CH3OH:NH4OH (65:25:4)
  6. 6
    기타evaporated
  7. 7
    기타dried in vacuo

실험 절차

1.37 gm (6 meq) of myristic acid and 972 mg (6 meq) of carbonyl diimidazole are combined in a minimum volume of tetrahydrofuran and reacted at room temperature for 1 hour. 0.8 Ml (6 meq+10%) of 3-dimethylaminopropylamine is added and reacted overnight at room temperature. The reaction mixture is evaporated under reduced pressure, dried in vacuo and the desired product purified by silica gel chromatography in the system CH2Cl2 :CH3OH:NH4OH (65:25:4). Fractions 53-65 are combined, evaporated and dried in vacuo to yield 325 mg of title compound having a m.p. of 46°-48° C. after recrystallization from acetone/water.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04824996uspto-grants-1989_04