反应详情

8 g of the trichloroethanone 3 prepared above are suspended in 150 ml of methanol, and 34 ml of hydrazine hydrate are slowly added dropwise at 5-10° C. When the addition is complete, the mixture is stirred at RT for a further 1 h. Half of the liquid components are subsequently removed in vacuo, and the residue is cooled to 0° C. The precipitating crystals are filtered off with suction and washed with methanol. The residue is subsequently dried at 80° C. in vacuo, giving 5.4 g of the hydrazide 4. HPLC-MS: Rt=1.263 min; [M+H+]: 257.1

1. additionWhen the addition
2. customHalf of the liquid components are subsequently removed in vacuo
3. temperaturethe residue is cooled to 0° C
4. filtrationThe precipitating crystals are filtered off with suction
5. washwashed with methanol
6. customThe residue is subsequently dried at 80° C. in vacuo