反应详情

Tetrabutylammonium bromide (1.7 g) was added to a stirred mixture of Intermediate 2 (2 g) and 4-chlorobenzyl bromide (2.4 g) in sodium hydroxide 20% aq. (14.2 mL) and Toluene (7 mL). The RM was stirred at room temp under nitrogen atm for 3 hours. An excess of sat NH4Cl aq. solution was added and the mixture was extracted with EtOAc (3×30 ml). The organics were combined, dried (hydrophobic frit) and concentrated under vacuum. The residue was purified on silica using a cyclohexane:ethyl acetate 0-100% gradient. The desired fractions were combined and concentrated under vacuum to give the title compound (1.5 g). LC/MS MH+ 317, Rt 1.91 min (5 minute run).

1. extractionthe mixture was extracted with EtOAc (3×30 ml)
2. customdried (hydrophobic frit)
3. concentrationconcentrated under vacuum
4. customThe residue was purified on silica using a cyclohexane
5. concentrationconcentrated under vacuum