HRID19968
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred suspension of 3-Methoxy-4-methanesulfonylamino-N-(3,4-methylenedioxyphenyl)benzamide (200 mg) in dry CH2Cl2 (20 ml) under nitrogen, was added boron tribromide (0.3 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-(3,4-dihydroxyphenyl)benzamide (DC51-DB) (65 mg, 34%) as pale brown crystals.
WORKUP
后处理
- customthe solvent evaporated in vacuo to a volume of 1 ml
- customPurification by column chromatography over silica gel eluting with chloroform
- additioncontaining methanol (10-20%)