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Benzonitrile, 2-broMo-4-hydrazinyl- synthesis

3synthesis methods
36282-26-5 Synthesis
2-Bromo-4-fluorobenzonitrile

36282-26-5
195 suppliers
$7.00/5g

Benzonitrile, 2-broMo-4-hydrazinyl-

263845-82-5
44 suppliers
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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