HRID241653
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
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
- temperaturewas refluxed for 6 h
- concentrationThe reaction mixture was concentrated in vacuo
- extractionextracted with ethyl acetate (20 mL) and water (30 mL)
- washThe organic layer was washed with water (20 mL) and brine (15 mL)
- dry with materialdried over magnesium sulfate
- customThe crude product (27 mg) was purified by prep LC-MS(“process A”)