반응 #2468008

ord-bbe8789f04bc4773a5970af04c4b6545

반응 방정식

COc1cnc(Cl)nc1Cl
2,4-dichloro-5-methoxy-pyrimidine
Cl.Cl.c1nc2c([nH]1)CCCN2
4,5,6,7-tetrahydroimidazopyridine dihydrochloride
CCN(C(C)C)C(C)C
ethyldiisopropylamine
COc1cnc(Cl)nc1N1CCc2nc[nH]c2C1
2-chloro-4-(3,4,6,7-tetrahydro-imidazo[4,5-c]pyridin-5-yl)-5-methoxy-pyrimidine

용매

반응 조건

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

후처리

  1. 1
    기타The crude mixture is purified by column chromatography
  2. 2
    workup.ADDITION0.2% formic acid is added to both eluants
  3. 3
    기타The suitable fractions are freeze-dried

실험 절차

1 g 2,4-dichloro-5-methoxy-pyrimidine are dissolved in 4 mL butanol and combined with 1.04 g 4,5,6,7-tetrahydroimidazopyridine dihydrochloride and 2.96 mL ethyldiisopropylamine. This mixture is stirred for 16 h at 50° C. and then the solvent is eliminated in vacuo. The crude mixture is purified by column chromatography. The carrier material used is C18-RP-silica gel and a gradient is run through which consists at the starting point of 95% water and 5% acetonitrile and at the finishing point of 70% water and 30% acetonitrile. 0.2% formic acid is added to both eluants. The suitable fractions are freeze-dried.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08258129B2uspto-grants-2012_09