تفاعل #1446080

معادلة التفاعل

dimethylthiourea

3-hydroxyl-2-butanone

→

1,3-dimethyl-4,5-dimethylimidazole-2-thione

المذيبات

1-hexanol

1-hexanol

ظروف التفاعل

المعالجة

1. 1
   أخرى1,3-dimethyl-4,5-dimethylimidazole-2-thione was synthesized
2. 2
   أخرىobtained
3. 3
   أخرىKuhn, et al. (N. Kuhn and T. Kratz, Synthesis, June 1993, p.561)
4. 4
   أخرىa procedure of synthesizing the
5. 5
   أخرىsubjected to a reflux reaction for about 12 hours
6. 6
   درجة الحرارةan increase in the reaction temperature
7. 7
   أخرىAfter a completion of the reflux reaction
8. 8
   أخرىto separate into a white solid component
9. 9
   أخرىThe yellow liquid component was removed by use of a syringe
10. 10
    غسيلthe remaining white solid component was rinsed with water and ether
11. 11
    أخرىdried

الإجراء التجريبي

1,3-dimethyl-4,5-dimethylimidazole-2-thione was synthesized according to a method obtained by modifying a method suggested by N. Kuhn, et al. (N. Kuhn and T. Kratz, Synthesis, June 1993, p.561), and a procedure of synthesizing the same is described below. 100 mmol of dimethylthiourea and 100 mmol of 3-hydroxyl-2-butanone were added to 250 ml of 1-hexanol in order, and then subjected to a reflux reaction for about 12 hours while increasing a reaction temperature to 150 to 160° C. At this time, white solid reactants were dissolved in 1-hexanol to be partly converted into yellow solid reactants according to an increase in the reaction temperature. After a completion of the reflux reaction, the resulting solution was left in a freezer at about −30° C. for about one day to separate into a white solid component and a yellow liquid component. The yellow liquid component was removed by use of a syringe, and the remaining white solid component was rinsed with water and ether and dried to produce 1,3-dimethyl-4,5-dimethylimidazole-2-thione. 1,3-dimethyl-4,5-dimethylimidazole-2-thione thus produced was analyzed by a 1H-NMR analyzer and the results are as follows:

المصدر