HRID703427

反应详情

EQUATION

反应方程式

HRID 703427 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Salicylamide (15.22 g), potassium hydroxide (85%, 7.73 g) and cyclopropylmethyl bromide (16.024 g) were heated together under reflux in absolute ethanol (100 ml) for 91/2 hours. The cooled mixture was filtered to remove inorganic products and the filtrate was evaporated to an oil. The oil was dissolved in 1:1 toluene:ethyl acetate (200 ml) and the solution was washed with 10% potassium hydroxide solution (2×30 ml), water (50 ml) and saturated brine (50 ml), dried (Na2SO4), and concentratred under reduced pressure, leaving 2-(cyclopropylmethoxy)benzamide as an oil which crystallised (17.606 g, 83%), mp 95°-100° C.

WORKUP

后处理

  1. filtrationThe cooled mixture was filtered
  2. customto remove inorganic products
  3. customthe filtrate was evaporated to an oil
  4. dissolutionThe oil was dissolved in 1:1 toluene
  5. washethyl acetate (200 ml) and the solution was washed with 10% potassium hydroxide solution (2×30 ml), water (50 ml) and saturated brine (50 ml)
  6. dry with materialdried (Na2SO4)