反応 #1885015

反応方程式

N-methyl-2-pyrrolidone

benzoyl chloride

4-iodobenzoylhydrazine

N-methyl-2-pyrrolidone

→

powdery white solid

収率 97.0%

1-benzoyl-2-(4-iodobenzoyl)hydrazine

収率 97.0%

溶媒

water

water

反応条件

後処理

1. 1
   その他Into a 300 mL three-neck flask was put
2. 2
   workup.STIRRINGthe solution was stirred at a room temperature for 18 hours
3. 3
   その他a solid was precipitated
4. 4
   ろ過The precipitated solid was collected by suction filtration
5. 5
   workup.ADDITIONThe collected solid was added into about 500 mL of a saturated aqueous solution of sodium hydrogen carbonate
6. 6
   workup.STIRRINGstirred
7. 7
   洗浄washed
8. 8
   ろ過After the washing, the mixture was subjected to suction filtration
9. 9
   その他to obtain a solid
10. 10
    workup.STIRRINGstirred
11. 11
    洗浄washed
12. 12
    ろ過After the washing, the mixture was subjected to suction filtration
13. 13
    その他to obtain a solid
14. 14
    洗浄The obtained solid was washed with methanol

実験手順

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%.

出典