تفاعل #51464

ord-5166686b963f4292b26369a10eef036a

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted three times with ethyl acetate
  2. 2
    غسيلThe combined organic layers were washed with brine
  3. 3
    تجفيفdried over MgSO4
  4. 4
    ترشيحThe reaction mixture was filtered
  5. 5
    أخرىall volatiles were removed under reduced pressure

الإجراء التجريبي

Imidazole (9.5 g, 140 mmol) was added in one portion to a solution of trichloropyrimidine (24.7 g, 135 mmol) and triethylamine (30 mL, 216 mmol) in THF (500 mL). After 16 hrs, the reaction mixture was poured into saturated, aqueous ammonium chloride and extracted three times with ethyl acetate. The combined organic layers were washed with brine and dried over MgSO4. The reaction mixture was filtered and all volatiles were removed under reduced pressure. 2-Imidazolyl-4,6-dichloropyrimidine (the compound of formula (VIIIa)) (9.61 g, 33%) was isolated by flash chromatography (20% ethyl acetate in hexane) as an off-white solid. 1H NMR: (CDCl3) δ 7.13 (s,1), 7.25 (s,1), 7.76 (s,1), 8.50 (s, 1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06849739B2uspto-grants-2005_02