HRID1926582

反应详情

EQUATION

反应方程式

HRID 1926582 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customThe solvents were evaporated
  2. customthe residue purified via reversed phase HPLC and fractions
  3. additioncontaining the product
  4. extractionthe aqueous layer extracted with dichloromethane
  5. dry with materialThe organic phase was then dried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated to dryness
  8. additionThe residue was treated with a solution 2N hydrochloric acid in diethyl ether
  9. customthe mixture evaporated to dryness