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
To (2-benzyloxycarbonylamino-3-m-tolyloxypropyl)carbamic acid tert-butyl ester (220 mg) obtained in Step 2 was added 4N solution (2 ml) of hydrogen chloride in dioxane, and the mixture was stirred at room temperature for 1 hr. The solvent was evaporated, dichloromethane (7 ml), benzoyl chloride (96 μl) and triethylamine (265 μl) were added to the obtained solid, and the mixture was stirred at room temperature for 1 hr. The reaction mixture was diluted with ethyl acetate and, after washing with water, the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained crude product was purified by silica gel chromatography (ethyl acetate-hexane) to give [1-(benzoylaminomethyl)-2-m-tolyloxyethyl]carbamic acid benzyl ester (200 mg).
WORKUP
后处理
- customThe solvent was evaporated
- additiondichloromethane (7 ml), benzoyl chloride (96 μl) and triethylamine (265 μl) were added to the obtained solid
- stirringthe mixture was stirred at room temperature for 1 hr
- additionThe reaction mixture was diluted with ethyl acetate
- washafter washing with water
- dry with materialthe organic layer was dried over anhydrous sodium sulfate
- customThe solvent was evaporated
- customthe obtained crude product
- customwas purified by silica gel chromatography (ethyl acetate-hexane)