反応 #658779

反応方程式

di-(2-aminopropyl)amine

Carbon disulfide

hydrogen sulfide

→

2,6-Dimethyl-2,3,5,6-tetrahydro-1H-imidazo[1,2-a]imidazole

溶媒

1-methylnaphthalene

反応条件

後処理

1. 1
   その他The solvent was then removed by distillation
2. 2
   workup.DISSOLUTIONThe product was then dissolved in approximately 5 mL of hexanes
3. 3
   workup.ADDITION0.5 mL of a 2.0 M ether solution of hydrogen chloride was added

実験手順

In a 100 mL flask, 0.4078 g of di-(2-aminopropyl)amine (0.00311 mol) was dissolved in 50 mL of 1-methylnaphthalene. Carbon disulfide (0.18 mL, 0.00298 mol) was added. The reaction was stirred for three hours then heated to 200° C. The reaction was heated for four days until production of hydrogen sulfide stopped. The solvent was then removed by distillation. The product was then dissolved in approximately 5 mL of hexanes and 0.5 mL of a 2.0 M ether solution of hydrogen chloride was added. The yield of the precipitate was 0.278 g (53%). The NMR had a doublet at 1.19 ppm, a multiplet at 3.44 ppm, a multiplet at 3.92 ppm and a multiplet at 4.15 ppm.

出典