تفاعل #70317

ord-e30161a12a854bb5a83611441302d0d4

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was evaporated
  2. 2
    workup.ADDITIONwater was added
  3. 3
    استخلاصextracted with CHCl3
  4. 4
    أخرىThe crude mixture was purified by chromatography over SiO2 eluting with DCM/MeOH mixtures

الإجراء التجريبي

A mixture of 2-(tert-butoxycarbonylamino)-5-(trifluoromethyl)benzoic acid (7.21 mmol, 2.2 g), H2SO4 (36 mmol, 1.92 ml) in ethanol (25 ml) was stirred at 100° C. for 16 hours. The solvent was evaporated, water was added, pH was taken to 6 and extracted with CHCl3. The crude mixture was purified by chromatography over SiO2 eluting with DCM/MeOH mixtures and affording 0.69 g (yield 41%) of the expected product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536165B2uspto-grants-2013_09