反应详情

To an ice-cooled stirred solution of (S)-3-amino-5-(4-methylpiperazin-1-yl)-3,4-dihydro-2H-1-benzopyran (230 mg, 0.930 mmol) and triethylamine (194 μL, 1.39 mmol) in anhydrous methylene chloride (10 mL) was added 2-furoyl chloride (101 μL, 1.02 mmol) under nitrogen. The ice-bath was removed, and the reaction mixture was allowed to reach room temperature. The mixture was washed with a 2 M NH3 solution, dried (MgSO4), and the solvent was removed in vacuo. The remains was purified on a chromatotron (accelerated thin layer chromatography, eluent: chloroform/ethanol; 92:8+0.5% conc. NH3) affording 249 mg (79% yield) of the title compound as a white solid: mp sinters >50° C.; [α]21D −83° (c 1.0, chloroform); EIMS (70 eV) m/z (relative intensity) 341 (52, M+).

1. customThe ice-bath was removed
2. customto reach room temperature
3. washThe mixture was washed with a 2 M NH3 solution
4. dry with materialdried (MgSO4)
5. customthe solvent was removed in vacuo
6. customThe remains was purified on a chromatotron (accelerated thin layer chromatography, eluent: chloroform/ethanol; 92:8+0.5% conc. NH3)