反応 #6867

ord-6cbd47be74554fafb353de8fa6d07f48

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGthe resulting mixture was stirred at room temperature for about 23 hours
  2. 2
    ろ過The product was filtered off
  3. 3
    洗浄washed with cold water (75 ml)
  4. 4
    その他triturated with p-dioxane (30 ml)
  5. 5
    ろ過The product was filtered off
  6. 6
    その他dried under reduced pressure

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07084135B1uspto-grants-2006_08