反应详情

To a solution of 5-isothiocyanato-1,3-dihydro-indol-2-one (2.3 g, 12.09 mmol) in dry dichloromethane (200 ml), 1,2-diamino-pyrazinium mesitylenate (5.21 g, 15.12 mmol), diisopropylethylamine (7.81 g, 60.45 mmol) and EDCl (4.63 g, 24.18 mmol) are added and stirred for 6 hours. The reaction mixture is concentrated and the residue is taken in water (100 ml), triturated and filtered, the crude solid is purified by silica column using (60-120) mesh to get the titled product as yellow solid (2.0 g, 55%); TLC: chloroform/methanol (9.5/0.5) Rf-0.3; HPLC purity (method A): 97%, Rt (min): 2.40; LCMS: mass found (M+, 301.0), Rt (min): 2.36;

1. concentrationThe reaction mixture is concentrated
2. customtriturated
3. filtrationfiltered
4. customthe crude solid is purified by silica column