HRID1930409
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
2-(4-Fluoro-2-methyl-5-nitrophenyl)acetic acid (18.43 g, 86.5 mmol, 1.00 eq) and cone. H2SO4 (4.00 ml) were combined in EtOH (300 ml) and stirred with heating at 85° C. After 2.5 h, the completed reaction was cooled to RT and concentrated as completely as possible. The residue was dissolved in MTBE (250 ml) and washed with H2O (2×) and brine (2×), dried (MgSO4), filtered and evaporated to afford ethyl 2-(4-fluoro-2-methyl-5-nitrophenyl)acetate (16.79 g, 81% yield) as a dark orange oil which was used as is in the next reaction. MS (ESI) m/z: 242.0 (M+H)+.
WORKUP
后处理
- customthe completed reaction
- temperaturewas cooled to RT
- concentrationconcentrated as completely as possible
- dissolutionThe residue was dissolved in MTBE (250 ml)
- washwashed with H2O (2×) and brine (2×)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated