تفاعل #46226

ord-ee956f20a69c48c28c18024ee16ef1fb

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe mixture was extracted with CH2Cl2 (3×)
  2. 2
    تجفيفThe organic phases were dried over Na2SO4
  3. 3
    أخرىevaporated under vacuum

الإجراء التجريبي

To N-(6-chloro-5-methyl-pyridin-2-yl)-2,2-dimethyl-propionamide (4.00 g, 17.7 mmol) was added 6 N HCl (20 mL) at room temperature. The mixture was stirred at 80° C. for 12 hours. The reaction mixture was basified with drop-wise addition of sat. NaHCO3 to pH 8-9, and then the mixture was extracted with CH2Cl2 (3×). The organic phases were dried over Na2SO4 and evaporated under vacuum to obtain the 6-chloro-5-methyl-pyridin-2-ylamine (900 mg, 36%). 1H NMR (400 MHz, CDCl3) δ 7.28 (d, J=8.0 Hz, 1H), 6.35 (d, J=8.0 Hz, 1H), 4.39 (br s, 2H), 2.22 (s, 3H). MS (ESI) m/z: 143 (M+H+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741321B2uspto-grants-2010_06