2-Fluorophenylhydrazine synthesis
- Product Name:2-Fluorophenylhydrazine
- CAS Number:2368-80-1
- Molecular formula:C6H7FN2
- Molecular Weight:126.13
Yield: 74%
Reaction Conditions:
with hydrogenchloride;sodium hydroxide;sodium hydrogen sulfate;sodium nitrite
Steps:
4 Preparation of 2-fluorophenylhydrazine with addition of n-butanol
Example 4 Preparation of 2-fluorophenylhydrazine with addition of n-butanol In a 2 l four-necked flask fitted with dropping funnel, stirrer and condenser, 240 g of HCl 30% strength and 180 g of n-butanol (saturated with water, approximately 80% strength) are initially charged. The solution is heated to 50° C. and, over a period of 25 minutes, admixed with a total of 1291 g of an aqueous solution of 2-fluorophenylhydrazinedisulfonate--prepared by diazotization of 111 g (1 mol) of 2-fluoroaniline (156 g of water, 303 g of HCl 30% strength, 170 g of NaNO2) and subsequent reduction with sulfite (560 g of NaHSO3 +100 g of NaOH). The reaction solution is kept at 50° C. for another 60 minutes. During the reaction, the reaction system forms two phases. The two phases are separated from one another in a 2 l separating funnel. The aqueous phase is subsequently extracted three times with 10 ml of n-butanol each time. The organic phases are combined and adjusted to pH 8.5 using aqueous sodium hydroxide solution (33% strength), and the aqueous phase that forms is also separated off. The solvent is subsequently concentrated until a viscous crystal slurry is formed. Yield: 98.2 g (0.74 mol) of 2-fluorophenylhydrazine (95% pure), this corresponds to a theoretical yield of 74.0%, based on the 2-fluoroaniline employed.
References:
Clariant GmbH US6057478, 2000, A
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