反应详情

温度

105 °C

About 200 mg of 1-(2,6-dimethylphenyl)-3-methylamidinourea hydrochloride was introduced in a gas chromatograph hypo vial and dissolved in 1 ml of acetonitrile. To the solution was added 0.2 ml of DMF DMA reagent. The vial was sealed with crimper and heated at 105° C. for 15 minutes in an oven. Seven vials were made. The contents of the vials were then put into a long-neck round bottom flask and evaporated to dryness by a flask evaporator. The solid mass was dissolved in a mixture of 30 ml of CHCl3 and 20 ml of water and shaken vigorously in a 60 ml separatory funnel. The aqueous layer was discarded and 20 ml of water was added and shaken. The CHCl3 layer was then taken and about 10 g of anhydrous Na2SO4 was added, the CHCl3 solution was decanted into a flask and evaporated to dryness. The solid material was dissolved in 2-pentanone (about 80 ml) at 70° C. The solution was concentrated and crystallized upon cooling. The crystals were collected and dried in a desiccator with P2O5 with vacuum for one hour.

1. customThe vial was sealed with crimper
2. customThe contents of the vials were then put into a long-neck round bottom flask
3. customevaporated to dryness by a flask
4. customevaporator
5. dissolutionThe solid mass was dissolved in a mixture of 30 ml of CHCl3 and 20 ml of water
6. addition20 ml of water was added
7. stirringshaken
8. additionabout 10 g of anhydrous Na2SO4 was added
9. customthe CHCl3 solution was decanted into a flask
10. customevaporated to dryness
11. dissolutionThe solid material was dissolved in 2-pentanone (about 80 ml) at 70° C
12. concentrationThe solution was concentrated
13. customcrystallized
14. temperatureupon cooling
15. customThe crystals were collected
16. dry with materialdried in a desiccator with P2O5 with vacuum for one hour