反应详情

) A solution of hydrazine (0.023 mol) and N,N-dimethyl-4-pyridinamine (catalytic quantity) in CH2Cl2 (50 ml) was cooled in an ice-water bath. Half of a solution of 4-benzoylbenzoyl chloride (0.023 mol) in CH2Cl2(60 ml) was added dropwise. The other half of this solution, and a solution of N,N-bis(1-methylethyl)ethanamine (0.023 mol) in CH2Cl2 (40 ml) were added simultaneously and dropwise. The resulting reaction mixture was stirred for 5 hours at RT. The crude reaction mixture was filtered and the filtrate was washed with water and extracted. The separated organic layer was dried (Na2SO4), filtered and the solvent was evaporated, yielding 1.9 g (34%) of 4-benzoylbenzoic acid hydrazide (interm. 12)

1. customThe resulting reaction mixture
2. customThe crude reaction mixture
3. filtrationwas filtered
4. washthe filtrate was washed with water
5. extractionextracted
6. dry with materialThe separated organic layer was dried (Na2SO4)
7. filtrationfiltered
8. customthe solvent was evaporated