HRID275237

反应详情

EQUATION

反应方程式

HRID 275237 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 500 ml RB flask containing a solution of lauroyl chloride (19.03 g., 87 mM) in dry chloroform (200 ml) was cooled to 0° C. on an ice bath. A solution of N, N-diethly-1,3-propanediamine (15.00 g., 115 mM) in dry chloroform (25 ml) was added dropwise to the cold solution then allowed to warm to room temperature and stirred for 2 hours. The chloroform was removed under reduced pressure and the residue redissolved in an ethanol/water mixture (1:1) and neutralized with sodium bicarbonate, followed by extraction with chloroform (4×50 ml). The combined extracts were dried (MgSO4), concentrated, and the residue distilled under reduced pressure (bp 176° C., 20μ) to give 21.47 g. (79%) of the subject compound as an amber oil.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. customThe chloroform was removed under reduced pressure
  3. dissolutionthe residue redissolved in an ethanol/water mixture (1:1)
  4. extractionfollowed by extraction with chloroform (4×50 ml)
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. concentrationconcentrated
  7. distillationthe residue distilled under reduced pressure (bp 176° C., 20μ)
  8. customto give 21.47 g