Benzoyl chloride → Benzoic acid, m-bromo-, benzoylhydrazide

Next, 5.0 grams (23 mmol) of the 3-bromobenzoylhydrazine obtained in (i) were placed into a 300 mL, three-neck flask, 10 mL of N-methyl-2-pyrrolidone was added thereto, and the mixture was stirred. A mixed solution of 10 mL of N-methyl-2-pyrrolidone and 3.2 mL (28 mmol) of benzoyl chloride were dripped into this mixture through a 50 mL dropping funnel. After completion of the dripping, the mixture was heated and stirred at 80° C. for 3 hours, and the contents of the flask were reacted together. After the reaction was completed, a solid was precipitated out with the addition of water to the reaction solution. A solid was obtained by suction filtration of the precipitate solid. The obtained solid was washed with approximately 1 L of water and removed by suction filtration. After the suction-filtered solid was washed with methanol and a solid was removed by suction filtration, 7.1 grams of a white-colored solid, which was the objective of the synthesis process, were obtained at a yield of 96%.

1. additionwas added
2. temperatureAfter completion of the dripping, the mixture was heated
3. stirringstirred at 80° C. for 3 hours
4. customthe contents of the flask were reacted together
5. customa solid was precipitated out with the addition of water to the reaction solution
6. customA solid was obtained by suction filtration of the precipitate solid
7. washThe obtained solid was washed with approximately 1 L of water
8. customremoved by suction filtration
9. washAfter the suction-filtered solid was washed with methanol
10. customa solid was removed by suction filtration, 7.1 grams of a white-colored solid, which
11. customwere obtained at a yield of 96%

ORDレコード

ord-3792f1be691042f3aac9c9884be17c84

出典データセット

uspto-grants-2012_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08221904B2