HRID1729248
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
4.2 ml of 1N sodium hydroxide was added dropwise under ice-cooling to a solution of 900 mg of methyl N-(9-fluorenylcarbonyl)glycinate in 55 ml of ethanol. The resultant mixture was stirred at room temperature for 1.5 hours. The residue obtained by concentrating the reaction mixture was dissolved in 0.5N sodium hydroxide, and washed with an ether. Under ice-cooling, the pH value of the aqueous layer was adjusted to 3 to 4 with 5% hydrochloric acid, and the precipitate formed was separated by filtration. The precipitate thus separated was washed with water and, then, recrystallized from a mixture of ethanol and ether to give 463 mg of N-(9-fluorenylcarbonyl)glycine as white needles.
WORKUP
后处理
- customThe residue obtained
- concentrationby concentrating the reaction mixture
- dissolutionwas dissolved in 0.5N sodium hydroxide
- washwashed with an ether
- temperatureUnder ice-cooling
- customthe precipitate formed
- customwas separated by filtration
- customThe precipitate thus separated
- washwas washed with water
- customrecrystallized from a mixture of ethanol and ether