HRID849394
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
Benzenesulphonamide (0.024 g, 0.13 mmol) was added to a solution of Example 26 (0.50 g, 0.12 mmol) and triethylamine (0.019 mL, 0.13 mmol) in CH2Cl2 (1 mL). After stirring for 16 hr, the reaction was diluted with CHCl3 (10 mL) and NaHCO3 (3 mL) and stirred for 30 min. The layers were separated and the aqueous layer was reextracted with CHCl3 (2×20 mL). The combined organic layers were dried over MgSO4, filtered and concentrated. The residue was treated with HCl/ether, a yellow solid was formed which was triturated with ether several times and dried under vacuum to afford Example 54 (0.64.2 g, 83%) as a light brown solid.
WORKUP
后处理
- stirringstirred for 30 min
- customThe layers were separated
- dry with materialThe combined organic layers were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- additionThe residue was treated with HCl/ether
- customa yellow solid was formed which
- customwas triturated with ether several times
- customdried under vacuum
- customto afford Example 54 (0.64.2 g, 83%) as a light brown solid