تفاعل #92062

ord-247f5cd8103c45698d5245051deb6a86

الكواشف

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المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe reaction mixture was concentrated
  2. 2
    أخرىpurified by column chromatography with gradient elution (petroleum ether: ethyl acetate=10:1 and dichloromethane)

الإجراء التجريبي

2-amino-4-trifluoromethylpyridine (5 g, 30.8 mmol, Langfang Beixin Chemical Co., Hebei) was dissolved in 100 mL of chloroform and N-bromosuccinimide (5.92 g, 33.3 mmol) was added in batches. The mixture was stirred in darkness or away from light at room temperature for 3 hours. The reaction mixture was concentrated and purified by column chromatography with gradient elution (petroleum ether: ethyl acetate=10:1 and dichloromethane), so as to give 4.33 g of red solid. Yield: 58.2%. LC-MS: 240 (M+1), 242 (M+2+1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09447101B2uspto-grants-2016_09