HRID1410519

反应详情

EQUATION

反应方程式

HRID 1410519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.50 g (0.82 mmol) N-(2,6-diisopropylphenyl)-4-(6-tosyloxy-1-hexinyl)-naphthaline-1,8-dicarboxylic acid imide and 0.36 g (5.5 mmol) sodium azide were stirred for 17 hours at room temperature under nitrogen atmosphere. 250 ml acetic acid and saturated sodium chloride solution were added to the reaction mixture. After mixing, the organic phase was removed and washed once with saturated sodium chloride solution and two times with water. The organic phase was dried with MgSO4 and the solvent was evaporated in a rotary evaporator at a temperature of the water-bath of 25° C. The obtained oil (0.40 g) was purified on silica gel ((60 Å, 60-200 μm) free flow agent: methylene chloride. 0.10 g (25% of the theoretical yield) of a orange-yellow solid material were obtained.

WORKUP

后处理

  1. additionAfter mixing
  2. customthe organic phase was removed
  3. washwashed once with saturated sodium chloride solution and two times with water
  4. dry with materialThe organic phase was dried with MgSO4
  5. customthe solvent was evaporated in a rotary evaporator at a temperature of the water-bath of 25° C
  6. customThe obtained oil (0.40 g) was purified on silica gel ((60 Å, 60-200 μm) free flow agent
  7. custom0.10 g (25% of the theoretical yield) of a orange-yellow solid material
  8. customwere obtained