تفاعل #52200

ord-f9f01c43aca840369211d72fc8d690c8

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux for 18 hours
  3. 3
    درجة الحرارةto cool
  4. 4
    أخرىthe volatiles were removed by evaporation
  5. 5
    أخرىThe residue was purified by chromatography
  6. 6
    غسيلeluting with ethyl acetate/hexane (50:50)
  7. 7
    درجة الحرارةincreasing in polarity to (70:30)

الإجراء التجريبي

A mixture of 2-methoxyethylamine (859 mg, 11.4 mmol), sulphanilyl fluoride (1.0 g, 5.71 mmol), and triethylamine (1.72 g, 22.9 mmol) in n-butanol (15 ml) was heated at reflux for 18 hours. The mixture was allowed to cool and the volatiles were removed by evaporation. The residue was purified by chromatography eluting with ethyl acetate/hexane (50:50) increasing in polarity to (70:30) to give the title compound (860 mg, 65%). NMR: 2.78 (q, 2H), 3.15 (s, 3H), 3.25 (t, 2H), 5.87 (s, 2H), 6.58 (d, 2H), 7.10 (t, 1H), 7.40 (d, 2H); m/z: 231 [MH]+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06855719B1uspto-grants-2005_02