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 mixture of methyl 4-(aminosulfonyl)benzoate (5.10 g) and potassium carbonate (6.55 g) in dimethoxyethane (50 mL) was refluxed for 5 minutes. After cooling the mixture, a solution of benzyl chloridocarbonate (5.25 g) in dimethoxyethane (30 mL), and the resulting mixture was refluxed for 1 hour. The reaction was quenched by adding 1N hydrochloric acid (100 mL). The mixture was extracted with ethyl acetate (200 mL), and the organic layer was washed with brine, dried over magnesium sulfate, and evaporated to give a pale yellow oil, which was solidified upon standing. The solid was triturated in diisopropyl ether (30 mL) to give methyl 4-({[(benzyloxy)carbonyl]amino}sulfonyl)benzoate as a white powder (3.38 g).
WORKUP
后处理
- temperaturewas refluxed for 5 minutes
- temperatureAfter cooling the mixture
- customThe reaction was quenched
- additionby adding 1N hydrochloric acid (100 mL)
- extractionThe mixture was extracted with ethyl acetate (200 mL)
- washthe organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- customevaporated
- customto give a pale yellow oil, which
- customThe solid was triturated in diisopropyl ether (30 mL)