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ChemicalBook CAS DataBase List 2-FLUORO-6-(TRIFLUOROMETHYL)BENZYLAMINE

2-FLUORO-6-(TRIFLUOROMETHYL)BENZYLAMINE synthesis

6synthesis methods
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Yield:239087-06-0 95%

Reaction Conditions:

Stage #1:2-fluoro-6-(trifluoromethyl)benzaldehyde with hydroxylamine hydrochloride;sodium hydroxide in ethanol;water for 1 h;
Stage #2: with hydrogenchloride;zinc in ethanol;water for 2 h;

Steps:

11-12 Example 12Preparation of 2-fluoro-6-trifluoromethylbenzylamine E6
Add 250 g of hydroxylamine hydrochloride and 50 ml of water to a 250 ml three-necked bottle.The aqueous phase was adjusted to neutrality with 10% sodium hydroxide, and then the ethanol solution of E5 (5g / 20ml) was slowly added dropwise. After stirring for 1h, 6g of zinc powder was added in batches.Hydrochloric acid (6 mol / L, 40 ml) was added dropwise. After 2 hours of reaction, the mixture was filtered, and 50 ml of ammonia was added to the filtrate.Adjust the pH to 11 with 6 ml of 33% sodium hydroxide, and extract with dichloromethane.The organic phase was collected, washed with saturated brine, and dried over anhydrous sodium sulfate.Suctioned and concentrated to give 4.78 g of yellow oil(95% yield).

References:

Shanghai Pharmaceutical Industry Institute;China Pharmaceutical Industry Zongyuan;Liu Yanming;Hao Qun;Lin Kuaile;Zhou Weicheng;Pan Jing;Chen Liang;Zhou Ting CN110498771, 2019, A Location in patent:Paragraph 0133-0136

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