반응 #595358

ord-a76f2533075a49bcb780ac35c9329078

반응 방정식

N#Cc1c(N)nc(S)c(C#N)c1-c1ccc(OCCO)cc1
compound
N#Cc1c(N)nc(S)c(C#N)c1-c1ccc(OCCO)cc1
2-Amino-4-[4-(2-hydroxyethoxy)phenyl]-6-mercaptopyridine-3,5-dicarbonitrile
Cc1cc(-c2nc(CCl)co2)ccc1Cl
compound
Cc1cc(-c2nc(CCl)co2)ccc1Cl
4-(Chloromethyl)-2-(4-chloro-3-methylphenyl)-1,3-oxazole
O=C([O-])O.[Na+]
sodium bicarbonate
Cc1cc(-c2nc(CSc3nc(N)c(C#N)c(-c4ccc(OCCO)cc4)c3C#N)co2)ccc1Cl
2-Amino-6-({[2-(4-chloro-3-methylphenyl)-1,3-oxazol-4-yl]methyl}thio)-4-[4-(2-hydroxyethoxy)-phenyl]pyridine-3,5-dicarbonitrile

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture is then filtered
  2. 2
    기타the filtrate is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)
  3. 3
    기타After removal of the solvent
  4. 4
    기타on a rotary evaporator
  5. 5
    기타the product is obtained as a white solid

실험 절차

52 mg (0.17 mmol) of the compound from Example 1A and 89 mg (0.18 mmol) of the compound from Example 28A, together with 42 mg (0.50 mmol) of sodium bicarbonate, are suspended in 1.8 ml of dry DMF. The reaction mixture is stirred at RT for 12 h. The mixture is then filtered and the filtrate is purified directly by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5). After removal of the solvent on a rotary evaporator, the product is obtained as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09095582B2uspto-grants-2015_08