HRID1794141

反应详情

EQUATION

反应方程式

HRID 1794141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (82 mg, 55%, 1.87 mM) was added to a solution of 3,5-difluoro-4-hydroxymethyl-phenol (300 mg, 1.87 mM) in dimethylformamide (4 mL). After 1 h stirring at room temperature cyclopropylmethylbromide (135 mg, 1.87 mM) was added and stirring continued for 24 h. The mixture was partitioned between water and diethylether. Organic phases were pooled, washed with brine and dried with MgSO4 to yield after evaporation a yellow oil (673 mg). This residue was purified by column chromatography (silica gel; n-hexane/ethylacetate gradient) to yield 287 mg (71%) of the product as a yellowish oil. MS (EI): 214.1 (M)+.

WORKUP

后处理

  1. additionwas added
  2. customThe mixture was partitioned between water and diethylether
  3. washwashed with brine
  4. dry with materialdried with MgSO4
  5. customto yield
  6. customafter evaporation a yellow oil (673 mg)
  7. customThis residue was purified by column chromatography (silica gel; n-hexane/ethylacetate gradient)