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
4-[5-(3-Difluoromethoxy-benzenesulfonylamino)-2-methyl-phenyl]-piperazine-1-carboxylic acid tert-butyl ester (0.097 g, 0.195 mmol) was dissolved in 5 mL of dichloromethane. A solution of 0.293 mL of 2N hydrochloric acid in diethyl ether was added and the mixture stirred for 16 h at room temperature. The solvents were evaporated, the residue purified via reversed phase HPLC and fractions containing the product were combined. The pH was adjusted to 9 with aqueous sodium bicarbonate and the aqueous layer extracted with dichloromethane. The organic phase was then dried over magnesium sulphate, filtered and evaporated to dryness. The residue was treated with a solution 2N hydrochloric acid in diethyl ether and the mixture evaporated to dryness to yield the title compound (0.017 mg).
WORKUP
后处理
- customThe solvents were evaporated
- customthe residue purified via reversed phase HPLC and fractions
- additioncontaining the product
- extractionthe aqueous layer extracted with dichloromethane
- dry with materialThe organic phase was then dried over magnesium sulphate
- filtrationfiltered
- customevaporated to dryness
- additionThe residue was treated with a solution 2N hydrochloric acid in diethyl ether
- customthe mixture evaporated to dryness