HRID241653

反应详情

EQUATION

反应方程式

HRID 241653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 1-(cyclopropylmethyl)-2-(2,2-dimethylpropyl)-5-[(piperidin-4-ylmethane)sulfonyl]-1,3-benzodiazole (STEP D of Example 5, 25 mg, 0.062 mmol), sulfamide (15 mg, 0.16 mmol)and 1,4-dioxane was refluxed for 6 h. The reaction mixture was concentrated in vacuo and extracted with ethyl acetate (20 mL) and water (30 mL). The organic layer was washed with water (20 mL) and brine (15 mL), dried over magnesium sulfate. The crude product (27 mg) was purified by prep LC-MS(“process A”).

WORKUP

后处理

  1. temperaturewas refluxed for 6 h
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. extractionextracted with ethyl acetate (20 mL) and water (30 mL)
  4. washThe organic layer was washed with water (20 mL) and brine (15 mL)
  5. dry with materialdried over magnesium sulfate
  6. customThe crude product (27 mg) was purified by prep LC-MS(“process A”)