HRID253695
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 a solution of methyl-6-chloro-3-(N-(4-ethylphenyl)-N′-hydroxycarbamimidoyl)-2-fluorobenzoate (225 mg, 641 μmol) in DMF (6.4 ml) chilled to 0° C. was added NaH (17 mg, 706 μmol) in one portion. The yellow solution evolved gas and immediately turned a dark orange color. After 20 min, the mixture was diluted with H2O and DCM, the layers were separated and the aqueous layer was extracted with DCM (2×). The organic layers were combined and washed with brine, dried over MgSO4, filtered and concentrated to provide the title compound as a light brown solid, which was used for the next step without further purification.
WORKUP
后处理
- customthe layers were separated
- extractionthe aqueous layer was extracted with DCM (2×)
- washwashed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated