反应详情

11.8 g (0.0375 mol) 2-Chloroethyl 2-(methoxyacetyl)-2-(2,6-dimethylphenyl)-hydrazinecarboxylate are added portion-wise to a suspension of 2.0 g sodium hydride (in form of about 55% by weight in mineral oil) in 100 ml absolute toluene at room temperature under a blanket of nitrogen. The reaction temperature rises gradually during this addition up to 40°. After the addtion is complete the mixture is stirred during 30 minutes without cooling and afterwards cooled to 10°. The unreacted sodium hydride is then destroyed with ethanol, the obtained solution washed with water dried with MgSO4 and the solvent removed in vacuo to give the end title compound which is recrystallised from ethanol to yield the title compound as colourless crystals, m.p. 103°-104°.

1. additionThe reaction temperature rises gradually during this addition up to 40°
2. temperaturewithout cooling
3. temperatureafterwards cooled to 10°
4. customThe unreacted sodium hydride is then destroyed with ethanol
5. washthe obtained solution washed with water
6. dry with materialdried with MgSO4
7. customthe solvent removed in vacuo