HRID1370499
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
A solution of 6-chloro-benzothiazol-2-ylamine (Example 200, 17.8 g, 96.7 mmol) and KOH (EM, 87 g, 1.55 mol) in 150 mL of water was refluxed for 2 d. The mixture was cooled to room temperature and was diluted with ice. The solution was brought to pH 5 with concentrated HCl. The mixture was extracted 3× with EtOAc (300 mL). The organic layers were combined and washed twice with a brine solution (300 mL), dried over Na2SO4. Removal of the solvent under reduced pressure gave 10.5 g product.
WORKUP
后处理
- additionwas diluted with ice
- extractionThe mixture was extracted 3× with EtOAc (300 mL)
- washwashed twice with a brine solution (300 mL)
- dry with materialdried over Na2SO4
- customRemoval of the solvent under reduced pressure