反应详情

A solution of t-butyl 1-piperazinecarboxylate 38 (1.0 g., 5.37 mmole), 3-chloro-4-fluoronitrobenzene (0.94 g., 5.37 mmole) and diisopropylethylamine (0.70 g., 5.4 mmole) in DMSO (30 mL.) was heated 16 hours at 100°, cooled to r.t. and poured into ice water (300 mL.). The suspension was extracted with ethyl acetate (2×60 mL.). The combined organic layers were washed with water (3×40 mL.), dried over Na2SO4 and evaporated to dryness to give an orange solid which was recrystallized twice from methanol to give the title compound, 1.2 g. MS (M+H)+ 342.0

1. extractionThe suspension was extracted with ethyl acetate (2×60 mL.)
2. washThe combined organic layers were washed with water (3×40 mL.)
3. dry with materialdried over Na2SO4
4. customevaporated to dryness
5. customto give an orange solid which
6. customwas recrystallized twice from methanol