反应详情

温度

0 °C

Methyl anthranilate (110 g, 0.73 mol) was dissolved in dichloromethane (1 liter) at 0° C. and triethylamine (115 ml, 0.8 mol) was added. Tosyl chloride (133 g, 0.745 mol) was added portionwise at 0° C. The reaction mixture was stirred for 30 min at 0° C. and 64 h at room temperature. The mixture was reduced in vacuo. The residue was dissolved in EtOAc and the organic layer was washed with 5% KHCO3 (aq) solution, 1N HCl solution and brine, dried, filtered and concentrated in vacuo. The residue was crystallised from EtOAc/hexane to yield the title compound (181 g, 81%).

1. washthe organic layer was washed with 5% KHCO3 (aq) solution, 1N HCl solution and brine
2. customdried
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was crystallised from EtOAc/hexane