ChemicalBook CAS DataBase List (3-CHLORO-PYRIDIN-2-YL)-HYDRAZINE

(3-CHLORO-PYRIDIN-2-YL)-HYDRAZINE synthesis

5synthesis methods

Product Name:(3-CHLORO-PYRIDIN-2-YL)-HYDRAZINE
CAS Number:22841-92-5
Molecular formula:C5H6ClN3
Molecular Weight:143.57

2, 3-dichloropyridine and hydrazine hydrate mix, add polar solvent, after back flow reaction 4-8 hour, reduce to the room temperature suction filtration promptly, yield of 3-chloro-2-hydrazino pyridine is 95%-99%.

2402-77-9 Synthesis

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Yield:22841-92-5 98.12%

Reaction Conditions:

with N-Methyldiethanolamine;hydrazine hydrate at 102 - 105; under 2250.23 - 3000.3 Torr; for 8 h;Inert atmosphere;Autoclave;Large scale;

Steps:

1 Example 1:
(1) In a 2000L closed glass-lined kettle, 900kg of methyldiethanolamine (99.05%, 7.48kmol), then add 220kg (3.52kmol) of 80% hydrazine hydrate, stir, add 500kg (99.1%, 2,3-dichloropyridine, 3.35kmol), pass nitrogen to 0.3~0.4MPa, turn off the nitrogen. Open the jacket steam of the reactor, raise the temperature, and keep it at 102~105C Warm the reaction for 8 hours, HPLC detects 0.28% of 2,3-dichloropyridine, and the reaction is complete. (2) Turn on the cooling water of the gas-phase three-stage condenser of the reactor, and turn on the water circulation in the tail gas falling film absorption tower. Slightly open Valve pressure relief, after pressure relief to normal pressure, the temperature is raised to 115~120C, and the nitrogen valve is opened at the same time, nitrogen is introduced into the reaction kettle, and bubbling and blowing off 30~60min. (3) After blowing off, the steam is turned off, the jacket of the reactor is cooled to normal temperature by steaming, and the material is discharged to the centrifuge for centrifugation. After drying and spinning, add water in a centrifuge to wash until the pH value of the effluent is 6.5~7. Centrifuge three times and use a total of 112 kg of washing water. Vacuum drying the centrifugal filter cake of step to obtain 460.7 kg of white needle-like crystalline powder, HPLC detection of 3-chloro- 2-hydrazinopyridine 99.21% (external standard method, the same below), the yield is 95.08%. (5) Collecting step (3) Synthetic liquid centrifugal filtrate (excluding water-washed filtrate), weighing 818.8 kg, and detecting 3 of them Chloro-2-hydrazinopyridine is 1.78%, of which 14.9kg 3-chloro-2-hydrazinopyridine is calculated, and the total yield is 98.12%.

References:

CN112694438, 2021, A Location in patent:Paragraph 0023; 0030-0034

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2402-77-9 Synthesis

2402-77-9
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$5.00/5g

22841-92-5
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References