تفاعل #6867

ord-6cbd47be74554fafb353de8fa6d07f48

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe resulting mixture was stirred at room temperature for about 23 hours
  2. 2
    ترشيحThe product was filtered off
  3. 3
    غسيلwashed with cold water (75 ml)
  4. 4
    أخرىtriturated with p-dioxane (30 ml)
  5. 5
    ترشيحThe product was filtered off
  6. 6
    أخرىdried under reduced pressure

الإجراء التجريبي

4-Hydroxymethylimidazole hydrochloride (compound xiii where R2 is H) (2.50 g, 18.6 mmol) and Et3N (2.59 ml, 18.6 mmol) were combined in DMF (30 ml) and stirred at room temperature. A solution of chlorotriphenylmethane (5.19 g, 18.6 mmol) in DMF (25 ml) was added dropwise at room temperature and the resulting mixture was stirred at room temperature for about 23 hours and then poured into ice water (300 ml). The product was filtered off, washed with cold water (75 ml) and triturated with p-dioxane (30 ml). The product was filtered off and dried under reduced pressure to yield product (4.96 g, 78%). NMR (300 MHZ, DMSO-d6, 30° C.) 7.3–7.5 (9H, m), 7.25–7.35 (1H, d), 7.0–7.2 (6H, m), 6.7–6.75 (1H, s), 4.15–4.2 (2H, m).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07084135B1uspto-grants-2006_08