Benzonitrile, 2-broMo-4-hydrazinyl- synthesis
- Product Name:Benzonitrile, 2-broMo-4-hydrazinyl-
- CAS Number:263845-82-5
- Molecular formula:C7H6BrN3
- Molecular Weight:212.05
36282-26-5
263845-82-5
Example 4a Preparation of 2-bromo-4-hydrazinobenzonitrile: Anhydrous hydrazine (10 mL) was slowly added to a solution of 2-bromo-4-fluorobenzonitrile (5.00 g, 25.00 mmol) in tetrahydrofuran (THF, 10 mL) through an addition funnel under dry conditions. After the addition was completed, the reaction mixture was stirred at room temperature for 24 hours. Upon completion of the reaction, water (20 mL) was added to the mixture to quench the reaction. The resulting white precipitate was collected by diafiltration and washed well with deionized water. Subsequently, the product was dried in a vacuum oven at 40 °C to afford 2-bromo-4-hydrazinylbenzonitrile (4.92 g, 93% yield) as a white solid. The structure of the product was confirmed by 1H NMR (300 MHz, CDCl3): δ 8.05 (br s, 1H), 7.47 (d, J = 8.7 Hz, 1H), 7.06 (d, J = 2.0 Hz, 1H), 6.72 (dd, J = 8.7, 2.0 Hz, 1H), 4.37 (br s, 2H); ESI MS m/z 212 [M + H]+.
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Yield:263845-82-5 93%
Reaction Conditions:
with hydrazine in tetrahydrofuran at 20; for 24 h;
Steps:
4.4a
Example 4a Preparation of 2-Bromo-4-hydrazino-benzonitrile To a solution of 2-bromo-4-fluorobenzonitrile (5.00 g, 25.00 mmol) in THF (10 mL) is added anhydrous hydrazine (10 mL) through an addition funnel. After addition, the resulting mixture is stirred at room temperature for 24 h. Water (20 mL) is added to the reaction mixture. A white precipitate is collected by filtration, washed with water, and dried in a vacuum oven at 40° C. to afford 2-Bromo-4-hydrazino-benzonitrile (4.92 g, 93%) as a white solid: 1H NMR (300 MHz, CDCl3) δ8.05 (br s, 1H), 7.47 (d, J=8.7 Hz, 1H), 7.06 (d, J=2.0 Hz, 1H), 6.72 (dd, J=8.7, 2.0 Hz, 1H), 4.37 (br s, 2H); ESI MS m/z 212 [M+H]+.
References:
US2008/119457,2008,A1 Location in patent:Page/Page column 45
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