HRID2304955

反应详情

EQUATION

反应方程式

HRID 2304955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 19.0 g aluminum chloride, dissolved in methylene chloride, was cooled to 0° C. and 46.5 g dodecylamine in methylene chloride was added dropwise (exothermic). At room temperature, 19.3 g gamma-undecalactone was added rapidly. The temperature rose to 36° C. The reaction was stirred at room temperature for 4 hours. The mixture was quenched with water and filtered over Celite. The liquid was extracted with ether and washed with water and brine. The solution was dried, filtered and evaporated to dryness. The resulting brown crystals were purified by recrystallization from ether/ethylacetate to give pale yellow crystals.

WORKUP

后处理

  1. customrose to 36° C
  2. customThe mixture was quenched with water
  3. filtrationfiltered over Celite
  4. extractionThe liquid was extracted with ether
  5. washwashed with water and brine
  6. customThe solution was dried
  7. filtrationfiltered
  8. customevaporated to dryness
  9. customThe resulting brown crystals were purified by recrystallization from ether/ethylacetate
  10. customto give pale yellow crystals