반응 #1905851

ord-f0d21cf4c9a648d88cf4eea650260c6a

용매

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the reaction was quenched with MeOH (2 mL)
  2. 2
    농축The reaction mixture was concentrated in vacuo
  3. 3
    기타purified by flash column chromatography
  4. 4
    세척eluted with a gradient of 0→5% CH3OH in CHCl3

실험 절차

5′-Amino-2′,5′-dideoxyuridine (0.237 g, 1.04 mmol) was reacted with 2-chlorotrityl chloride (0.415 g, 1.33 mmol) in dry pyridine (5 mL) at 40° C. for 24 h. A second portion of 2-chlorotrityl chloride (0.198 g, 0.63 mmol) was added. After a further 2 h stirring at 40° C., the reaction was quenched with MeOH (2 mL). The reaction mixture was concentrated in vacuo and purified by flash column chromatography using an ISOLUTE Si column eluted with a gradient of 0→5% CH3OH in CHCl3. The fractions with Rf=0.17 (10% CH3OH/CHCl3) yielded the title compound as a white solid (85 mg, 16%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07601702B2uspto-grants-2009_10