HRID893263

反应详情

EQUATION

反应方程式

HRID 893263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

Into a 100 ml round-bottomed flask, equipped with a magnetic stirrer and heating bath, were placed 2.4 g (0.02 mol) of dithiooxamide, 1.8 g (0.02 mol) of aniline, and 40 ml of methanol. The solution was stirred and heated at 35° C. for 30 minutes. The reactive amine, dodecylamine (3.7 g, 0.02 mol), was then added, and the solution was stirred for an additional 3 hours at 35° C. The crude reaction mixture was cooled to 25° C., and the acidity was adjusted to a pH of about 2 by the addition of 37% aqueous HCl. The mixture was filtered, washed with a small amount of methanol, and dried to afford 1.5 g of N,N'-didodecyldithiooxamide. Water (40 ml) was added to the filtrate with stirring, which was continued for 10 minutes. The precipitate was collected by filtration and washed with a minimum amount of a 50:50 mixture of water and methanol. The product was dried to afford 3.2 g (55%) of N-dodecyldithiooxamide.

WORKUP

后处理

  1. customInto a 100 ml round-bottomed flask, equipped with a magnetic stirrer
  2. temperatureheating bath
  3. stirringthe solution was stirred for an additional 3 hours at 35° C
  4. customThe crude reaction mixture
  5. temperaturewas cooled to 25° C.
  6. filtrationThe mixture was filtered
  7. washwashed with a small amount of methanol
  8. customdried