HRID1444560

反应详情

EQUATION

反应方程式

HRID 1444560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of the 3,5,5-trimethylhexanal (17.4 mL, 0.10 mol), ammonium chloride (53.5 g, 0.205 mol) and diethyl ether (113 mL) was added sodium cyanide (7.35 g, 0.15 mol) in water (38 mL). The reaction mixture was allowed to stir vigorously for 16 h. The layers were separated. The aqueous layer was extracted with diethyl ether. The combined organic layer was then extracted with 1 N HCl. Saturated sodium bicarbonate was then added until 1-cyano-3,5,5-trimethyl-hexylamine was completely precipitated. Vacuum filtration and washing with 5 mL ice cold water followed by lyophilization gave 1-cyano-3,5,5-trimethylhexylamine (5.805 g, 0.034 mol, 34.5%) as a white solid.

WORKUP

后处理

  1. customThe layers were separated
  2. extractionThe aqueous layer was extracted with diethyl ether
  3. extractionThe combined organic layer was then extracted with 1 N HCl
  4. additionSaturated sodium bicarbonate was then added until 1-cyano-3,5,5-trimethyl-hexylamine
  5. customwas completely precipitated
  6. filtrationVacuum filtration
  7. washwashing with 5 mL ice cold water