HRID1872687
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 an ice cold solution of 4-chloro-2-methoxybenzoic acid (1.0 g, 5.36 mmol) in trifluoroacetic acid (7 ml) was added N-chloromorpholine (0.67 g, 5.5 mmol) dropwise, maintaining the internal temperature below 10° C. After stirring overnight at room temperature the trifluoroacetic acid was removed in vacuo and the residue partitioned between ethyl acethate and water. The organic layer was dried over magnesium sulfate, concentrated in vacuo and the residue recrystallised from methanol to afford the title compound as a white solid (200 mg).
WORKUP
后处理
- temperaturemaintaining the internal temperature below 10° C
- customwas removed in vacuo
- customthe residue partitioned between ethyl acethate and water
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationconcentrated in vacuo
- customthe residue recrystallised from methanol