HRID23123
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 the product from Step A (0.0119 moles) was added 150 mL of CH2Cl2, one drop of DMF, 10 mL of oxalyl chloride, and the mixture was stirred at room temperature for 3 hours. After cooling to 10° C., 30 mL of NH4OH (exothermic) was added and the mixture was stirred for 30 min. The reaction mixture was then concentrated and the resulting residue diluted with ethyl acetate. The organic layer was washed with 1N NaOH, brine, dried over Na2SO4, and concentrated to give the 3-(benzyl)benzamide as a white solid. which was used without further purification.
WORKUP
后处理
- temperatureAfter cooling to 10° C.
- stirringthe mixture was stirred for 30 min
- concentrationThe reaction mixture was then concentrated
- additionthe resulting residue diluted with ethyl acetate
- washThe organic layer was washed with 1N NaOH, brine
- dry with materialdried over Na2SO4
- concentrationconcentrated