反应详情

To a suspension of 12.21 g. (0.05 moles) of methyl guanidine sulfate in 110 ml. of tetrahydrofuran is added 8.0 g. (0.10 moles of sodium hydroxide) of 50% aqueous sodium hydroxide. After stirring for 11/2 hours, 4.5 g. of sodium sulfate is slowly added and the mixture stirred an additional 1/2 hour. To the solution is added a solution of 9.88 g. (0.05 moles) of 2,6-dimethylphenyl-N-methylcarbamoyl chloride in 30 ml. of tetrahydrofuran. After stirring for 24 hours, the THF is removed in vacuo and the residue partitioned with chloroform/water. The oily residue is triturated with 300 ml. of hexane and 20 ml. benzene to give a white solid. This is dissolved in 50 ml. of 1:4 HNO3 and warmed slightly over 1/2 hour, then cooled. The white solid which forms is filtered and air dried to obtain 1-(2',6'-dimethylphenyl)-1-methyl-3-methylamidinourea nitrate.

1. additionTo a suspension of 12.21 g
2. stirringthe mixture stirred an additional 1/2 hour
3. additionTo the solution is added a solution of 9.88 g
4. stirringAfter stirring for 24 hours
5. customthe THF is removed in vacuo
6. customthe residue partitioned with chloroform/water
7. customThe oily residue is triturated with 300 ml
8. custombenzene to give a white solid
9. dissolutionThis is dissolved in 50 ml
10. temperaturecooled
11. filtrationThe white solid which forms is filtered
12. customair dried