반응 #1462117

ord-c3aeca193e994a63bdcf8639e98baea9

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heating
  2. 2
    workup.WAITto stand at room temperature overnight
  3. 3
    여과The product was recovered by filtration
  4. 4
    세척washed with a mixture of tert-butyl methyl ether and acetonitrile (7:3 v/v, 50 mL)
  5. 5
    기타The crude product was recrystallized from a mixture of acetonitrile and tert-butyl methyl ether

실험 절차

A mixture of N-(chloroacetyl)pyrrolidine (2.0 g, 13.55 mmol) and 1,2-dimethylimidazole (1.3 g, 13.5 mmol) were heated neat at 110° C. for 3 hours. To the reaction mixture was added acetonitrile (5 mL), and heating was continued for 20 minutes. Tert-butyl methylether (10 mL) was added, and the resulting mixture was allowed to stand at room temperature overnight. The product was recovered by filtration, and washed with a mixture of tert-butyl methyl ether and acetonitrile (7:3 v/v, 50 mL). The crude product was recrystallized from a mixture of acetonitrile and tert-butyl methyl ether to obtain 1.23 g (41%) of a white solid; mp 191–193° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07166625B2uspto-grants-2007_01