反应详情

温度

105 °C

About 200 mg. of 1-(2',6'-dimethylphenyl)-3-methylamidinourea is introduced into a gas chromatograph hypo vial and dissolved in 1 ml. of acetonitrile. To the solution is added 0.2 ml. of DMF DMA reagent. The vial is sealed with crimper and heated at 105° C. for 15 minutes in an oven. Seven vials are made. The contents of the vials are then put into a long-neck round bottom flask and evaporated to dryness by a flask evaporator. The solid mass is dissolved in a mixture of 30 ml. of CH Cl3 and 20 ml. of water and shaken vigorously in a 60 ml. separatory funnel. The aqueous layer is discarded and 20 ml. of water is added and shaken. The CH Cl3 layer is then taken off and about 10 g. of anhydrous Na2SO4 is added, the CH Cl3 solution is decanted into a flask and evaporated to a dryness. The solid material is dissolved in pentanone-2 (about 80 ml.) at 70° C. The solution is concentrated and crystallizes upon cooling. The crystals are collected and dried in a desiccator with P2O5 with vacuum for one hour.

1. dissolutiondissolved in 1 ml
2. additionTo the solution is added 0.2 ml
3. customThe vial is sealed with crimper
4. customThe contents of the vials are then put into a long-neck round bottom flask
5. customevaporated to dryness by a flask
6. customevaporator
7. dissolutionThe solid mass is dissolved in a mixture of 30 ml
8. additionof water is added
9. stirringshaken
10. additionof anhydrous Na2SO4 is added
11. customthe CH Cl3 solution is decanted into a flask
12. customevaporated to a dryness
13. dissolutionThe solid material is dissolved in pentanone-2 (about 80 ml.) at 70° C
14. concentrationThe solution is concentrated
15. customcrystallizes
16. temperatureupon cooling
17. customThe crystals are collected
18. dry with materialdried in a desiccator with P2O5 with vacuum for one hour