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
Under a nitrogen atmosphere, 10% Pd—C (1.0 g) was added to a solution of 3-nitro-o-cresol (10.0 g, 65.3 mmol) in methanol (200 ml) at room temperature, and catalytic reduction was carried out at ordinary temperature and atmospheric pressure. After completion of the reaction, the catalyst was filtered off and the filtrate was concentrated under reduced pressure. The resulting residue was dissolved in ethyl acetate, followed by adding thereto acetic anhydride (10.0 ml, 170 mmol) and pyridine (10.6 ml, 131 mmol), and the resulting mixture was refluxed for 2 hours. After completion of the reaction, the reaction mixture was concentrated and hexane was added thereto. The resulting suspension was filtered and the precipitate was dried under reduced pressure to obtain 3-(acetylamino)-2-methylphenyl acetate (12.7 g, 94%).
WORKUP
后处理
- customAfter completion of the reaction
- filtrationthe catalyst was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- dissolutionThe resulting residue was dissolved in ethyl acetate
- additionby adding
- customAfter completion of the reaction
- concentrationthe reaction mixture was concentrated
- additionhexane was added
- filtrationThe resulting suspension was filtered
- customthe precipitate was dried under reduced pressure