Benzoyl chloride → 1-Benzoyl-2-(4-iodobenzoyl)hydrazine

Into a 300 mL three-neck flask was put 15 g (57 mmol) of 4-iodobenzoylhydrazine, 15 mL of N-methyl-2-pyrrolidone (NMP) was added thereto, and the mixture was stirred for 10 minutes at a room temperature. After the stirring, 50 mL of a mixed solution of 5 mL of N-methyl-2-pyrrolidone and 7.9 mL (69 mmol) of benzoyl chloride was dripped into the solution through a dropping funnel, and the solution was stirred at a room temperature for 18 hours. After the stirring, water was added into the solution, and a solid was precipitated. The precipitated solid was collected by suction filtration. The collected solid was added into about 500 mL of a saturated aqueous solution of sodium hydrogen carbonate, stirred, and washed. After the washing, the mixture was subjected to suction filtration to obtain a solid. The obtained solid was added into about 500 mL of water, stirred, and washed. After the washing, the mixture was subjected to suction filtration to obtain a solid. The obtained solid was washed with methanol to give 20 g of a powdery white solid in a yield of 97%.

1. customInto a 300 mL three-neck flask was put
2. stirringthe solution was stirred at a room temperature for 18 hours
3. customa solid was precipitated
4. filtrationThe precipitated solid was collected by suction filtration
5. additionThe collected solid was added into about 500 mL of a saturated aqueous solution of sodium hydrogen carbonate
6. stirringstirred
7. washwashed
8. filtrationAfter the washing, the mixture was subjected to suction filtration
9. customto obtain a solid
10. stirringstirred
11. washwashed
12. filtrationAfter the washing, the mixture was subjected to suction filtration
13. customto obtain a solid
14. washThe obtained solid was washed with methanol

ORD-Eintrag

ord-f0ece7b2d05d4470964092363d930256

Quelldatensatz

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08343639B2