反应详情

To a 20 ml scintillation vial was added 2,3-dichloro-5-(chlorosulfonyl)benzoic acid (170 mg, 0.587 mmol). To this was added 1.5 ml of DCM and 7 ml of 7M NH4OH. The reaction mixture was stirred vigorously at room temperature overnight. After consumption of the starting material, the reaction solution was concentrated to half volume with a rotary evaporator and acidified with 6M HCl to ˜pH 4.5. The resulting solution was left at room temperature until the product precipitated. The product was collected by vacuum filtration and air dried, yielding 5-(aminosulfonyl)-2,3-dichlorobenzoic acid (80 mg, 50%) as light yellow solid.

1. customAfter consumption of the starting material
2. concentrationthe reaction solution was concentrated to half volume with a rotary evaporator
3. waitThe resulting solution was left at room temperature until the product
4. customprecipitated
5. filtrationThe product was collected by vacuum filtration and air
6. customdried