反应详情

温度

85 °C

A mixture of 4-chlorophenylacetyl chloride (1.36 g, 7.22 mmol) (Aldrich), 3-hydroxy-4-methyl-benzoic acid hydrazide (1.0 g, 6.02 mmol) (from Example 6 supra) and triethylamine (1.36 mL) in tetrahydrofuran (20 mL) was heated at 85° C. for 1 day. The reaction mixture was partitioned between ethyl acetate and water. The aqueous phase was extracted with ethyl acetate (1×). The combined organic phase washed with water and brine, dried (magnesium sulfate) and concentrated. The residue washed with ethyl acetate and dichloromethane and dried to give 3-hydroxy-4-methyl-benzoic acid N′-[2-(4-chloro-phenyl)-acetyl]-hydrazide. (Yield 0.91 g, 95%).

1. customThe reaction mixture was partitioned between ethyl acetate and water
2. extractionThe aqueous phase was extracted with ethyl acetate (1×)
3. washThe combined organic phase washed with water and brine
4. dry with materialdried (magnesium sulfate)
5. concentrationconcentrated
6. washThe residue washed with ethyl acetate and dichloromethane
7. customdried