تفاعل #1994287

ord-e86de8df2a6547c6adc88e09636516d6

معادلة التفاعل

[Cl][Sn][Cl]
Tin (II) chloride
O=[N+]([O-])c1cc(Cl)c(Cl)cc1F
1,2-dichloro-4-fluoro-5-nitrobenzene
O=C([O-])O.[Na+]
sodium bicarbonate
Nc1cc(Cl)c(Cl)cc1F
title compound
Nc1cc(Cl)c(Cl)cc1F
4,5-Dichloro-2-fluorophenylamine

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto near reflux during the addition
  2. 2
    درجة الحرارةupon cooling
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلThe organic phase was washed several more times with water
  5. 5
    أخرىdried
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated

الإجراء التجريبي

Tin (II) chloride dehydrate (27.0 g, 119.6 mmol) was dissolved in ethanol and 1,2-dichloro-4-fluoro-5-nitrobenzene (5.0 g, 23.8 mmol) was added dropwise. Temperature rose to near reflux during the addition and was complete upon cooling. The reaction mixture was carefully added to saturated aqueous sodium bicarbonate and then extracted with ethyl acetate. The organic phase was washed several more times with water, dried, filtered and concentrated to give the title compound as a yellow solid: 1H NMR (CDCl3): δ 7.17 (d, 1H), 6.84 (d, 1H), 3.78 (br s, 2H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08598085B2uspto-grants-2013_12