تفاعل #8516

ord-9a91687510384f2a99c8906dc00af77d

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe cooled mixture was evaporated
  2. 2
    استخلاصthe residue extracted with cyclohexane
  3. 3
    أخرىevaporated

الإجراء التجريبي

Phosphoryl chloride (500 microlitres, 1.7 equivalents) was added in one portion to a stirred solution of N′-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide (1.0 g, 3.11 mmol) in toluene (20 ml) and heated at 70° C. under an argon atmosphere for 20 hours. The cooled mixture was evaporated and the residue extracted with cyclohexane. The extracts were combined and evaporated to give the title compound (0.971 g) as an orange oil, NMR 4.4 (s, 2H), 7.55 (s, 2H), 7.7 (s, 1H). The yield was 90%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07087786B2uspto-grants-2006_08