تفاعل #513402

ord-9e66d77aa11046c4b33a23e0e82cf8e4

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 24 hr
  2. 2
    ترشيحthe mixture was filtered
  3. 3
    أخرىevaporated in vacuo
  4. 4
    أخرىThe residue was purified by silica gel column chromatography (eluent, from hexane to 2% ether in hexane)

الإجراء التجريبي

A mixture of 2,4-dichloro-6-methylpyrimidine (12.5 g, 76.65 mmol), N-chloro succinimide (12.28 g, 92 mmol), and benzoyl peroxide (2.78 g, 11.5 mmol) in carbon tetrachloride (150 ml) was refluxed for 24 hr. After cooling to room temperature, the mixture was filtered and evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, from hexane to 2% ether in hexane) to afford 6 g (40%) of 2,4-dichloro-6-chloromethyl-pyrimidine as a white solid. 1H NMR (200 MHz, CDCl3) δ 4.58 (2H, s), 7.55 (1H, s).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08106064B2uspto-grants-2012_01