HRID606675

反应详情

EQUATION

反应方程式

HRID 606675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

49.0 g (334 mmol) 2-cyanobenzeneboronic acid and 25.9 g (340 mmol) 1,3-propanediol were dissolved in 1 L CH2Cl2 with stirring in a 2 L round bottom flask for 20 h. The solution was then poured over a filter with suction to remove gummy solids. The filtrate was then dried with anhydrous MgSO4 to remove residual water, filtered and evaporated of solvent to give light-colored oil. The oil was then dissolved in CH2Cl2 and purified on a silica gel plug using CH2Cl2 as eluent. The product fractions were evaporated down to give the product as clear oil (35.7 g, 57.2% yield).

WORKUP

后处理

  1. additionThe solution was then poured over
  2. filtrationa filter with suction
  3. customto remove gummy solids
  4. dry with materialThe filtrate was then dried with anhydrous MgSO4
  5. customto remove residual water
  6. filtrationfiltered
  7. customevaporated of solvent
  8. customto give light-colored oil
  9. custompurified on a silica gel plug
  10. customThe product fractions were evaporated down