反应详情

A mixture of 1-acetyl-6-amino-4-phenyl-1,2,3,4-tetrahydro-2,2,4-trimethylquinoline (10 mg), 4-chlorobenzoyl chloride (11 mg) and N,N-diisopropylethylamine (22 μl) in tetrahydrofuran (1 ml) was stirred for 18 h. The reaction mixture was concentrated in vacuo, the residue was dissolved in ethyl acetate and washed with 0.5HCl, water, 5% aq. NaHCO3, water and brine. The organic layer was separated, dried (MgSO4) and concentrated in vacuo. The residue was chromatographed on silicagel in heptane/ethyl acetate=1/0=>0/1 (v/v) as eluent.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionthe residue was dissolved in ethyl acetate
3. washwashed with 0.5HCl, water, 5% aq. NaHCO3, water and brine
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe residue was chromatographed on silicagel in heptane/ethyl acetate=1/0=>0/1 (v/v) as eluent