HRID253695

反应详情

EQUATION

反应方程式

HRID 253695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. customthe layers were separated
  2. extractionthe aqueous layer was extracted with DCM (2×)
  3. washwashed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated