Benzoyl chloride → N'-benzoyl-4-bromobenzohydrazide

2.0 g (13.9 mmol) of 4-bromobenzoylhydrazine was put into a 300 mL three-neck flask, 7 mL of N-methyl-2-pyrrolidone was added thereto, and the mixture was stirred at a room temperature. A mixed solution of 5.0 mL of N-methyl-2-pyrrolidone and 2.5 mL (21.5 mmol) of benzoyl chloride was dripped into the solution through a 50 mL dropping funnel. The mixture was stirred at 80° C. for 3 hours. After the reaction, a solid was precipitated out with the addition of the reactive mixture to approximately 200 mL of water. The precipitated solid was collected by suction filtration. The collected solid was washed with water, a saturated sodium hydrogen carbonate solution, and saturated saline, in the order given. The obtained solid was recrystallized with a mixed solvent of acetate and hexane, so that 3.6 g of a white solid, which was the object of the synthesis, was obtained at a yield of 80%.

1. stirringThe mixture was stirred at 80° C. for 3 hours
2. customAfter the reaction
3. customa solid was precipitated out with the addition of the reactive mixture to approximately 200 mL of water
4. filtrationThe precipitated solid was collected by suction filtration
5. washThe collected solid was washed with water
6. customThe obtained solid was recrystallized with a mixed solvent of acetate and hexane, so that 3.6 g of a white solid, which
7. customthe object of the synthesis
8. customwas obtained at a yield of 80%

ORDレコード

ord-534d66e8730646ff88a3c45405532466

出典データセット

uspto-grants-2013_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08592056B2