反应详情

To a stirred suspension of 4-methanesulfonylamino-3-methoxy-N-(3-methanesulfonylamino-4-methoxyphenyl)benzamide (1.25 g) in dry CH2Cl2 (50 ml) under nitrogen, was added boron tribromide (1.5 ml) then stirring continued for a further 20 hours. Methanol (50 ml) was added carefully, then the solvent evaporated in vacuo to a volume of 1 ml, this was repeated 2 more times. Purification by column chromatography over silica gel eluting with chloroform containing methanol (10-20%) gave 3-hydroxy-4-methanesulfonylamino-N-(3-methanesulfonylamino-4-hydroxyphenyl)benzamide (143 mg, 15%) as an off-white solid.

1. customthe solvent evaporated in vacuo to a volume of 1 ml
2. customPurification by column chromatography over silica gel eluting with chloroform
3. additioncontaining methanol (10-20%)