HRID554559

反应详情

EQUATION

反应方程式

HRID 554559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a nitrogen stream, a boron trichloride methylene chloride solution (1.0 M, 6.4 mL, 6.4 mmol) was added to a solution of (4-cyclopropylphenyl)-(3-methoxy-5-methylthiophen-2-yl)methanone (582 mg, 2.14 mmol) in methylene chloride (12 mL) at −15° C. and the reaction mixture was stirred for one hour. Water was added thereto and the mixture was extracted with methylene chloride. The organic layer was washed with a saturated sodium chloride aqueous solution and dried (anhydrous magnesium sulfate), and then the solvent was distilled under reduced pressure. The obtained residue was purified by silica gel column chromatography [developing solution=methanol:methylene chloride (1:100)] to obtain the title compound (497 mg, 90%).

WORKUP

后处理

  1. extractionthe mixture was extracted with methylene chloride
  2. washThe organic layer was washed with a saturated sodium chloride aqueous solution
  3. dry with materialdried (anhydrous magnesium sulfate)
  4. distillationthe solvent was distilled under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography [developing solution=methanol:methylene chloride (1:100)]