反应详情

温度

65 °C

To a mixture of 1-(4-chlorobenzyl)-1-[4-(quinolin-2-ylmethoxy)phenyl]hydrazine from Example 1A, Step D, (660 mg, 1.7 mmol) and anhydrous NaOAc (160 mg, 1.95 mmol) in toluene (3 mL) was added glacial HOAc (1.5 mL). After 30 minutes, a solution containing methyl 5-(t-butylthio)-2,2-diethyl-4-oxopentanoate from Step B (402 mg, 1.47 mmol) in toluene (1 mL) was added and the reaction mixture stirred for 24 hours at room temperature and for 48 hours at 65° C. The reaction was then diluted with EtOAc, washed with NH4OAc buffer (25% w/v) and dried over MgSO4. Filtration and concentration gave a viscous oil which was purified by flash chromatography on silica gel (eluant: EtOAc-hexane 15:85) to give the title compound.

1. additionwas added
2. washwashed with NH4OAc buffer (25% w/v)
3. dry with materialdried over MgSO4
4. filtrationFiltration and concentration
5. customgave a viscous oil which
6. customwas purified by flash chromatography on silica gel (eluant: EtOAc-hexane 15:85)