反应详情

温度

45 °C

To a solution of 2-methyl-3-nitrobenzothioamide (2.50 g, 12.74 mmol) in ethanol (50 mL) at rt was added hydrazine, H2O (12.49 mL, 255 mmol). The mixture was heated at 45° C. for 4 hr and then concentrated under vacuum to a volume of approximately 20 mL. The residue was diluted with water (20 mL) and extracted with CH2Cl2 (5×50 mL). The combined extract was dried over anhydrous MgSO4. Removal of solvent under vacuum provide the desired product, 2-methyl-3-nitrobenzimidohydrazide (2.12 g, 10.92 mmol, 86% yield), as a white solid.

1. concentrationconcentrated under vacuum to a volume of approximately 20 mL
2. additionThe residue was diluted with water (20 mL)
3. extractionextracted with CH2Cl2 (5×50 mL)
4. extractionThe combined extract
5. dry with materialwas dried over anhydrous MgSO4
6. customRemoval of solvent under vacuum