반응 #8902

ord-1947bd8bee374badb21ae13f23022d0b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with saturated NaCl/NaHCO3 solution (1:1)
  2. 2
    기타The residue from the concentrated solution was purified via silica gel flash chromatography
  3. 3
    세척eluting with a gradient of 0 to 75% ethyl acetate/hexane

실험 절차

To a solution of 0.5 g (1.46 mmol) of the product of Step B in 10 mL DMF was added 0.954 g Cs2CO3 and 0.197 mL of 1-bromopinacolone. The reaction was stirred 17 hours at room temperature at which point the reaction mixture was diluted with ethyl acetate and washed with saturated NaCl/NaHCO3 solution (1:1). The residue from the concentrated solution was purified via silica gel flash chromatography eluting with a gradient of 0 to 75% ethyl acetate/hexane to afford the title compound. HPLC-MS: 439.1 (M+1), 441.1 (M+3); Rt=4.53 min.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091216B2uspto-grants-2006_08