반응 #44504

ord-84851ac9e32e4a5d977463b84fec4a0b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction was partitioned between ethyl acetate and water
  2. 2
    세척The organic layer was washed with brine (25 mL)
  3. 3
    건조dried with MgSO4
  4. 4
    여과filtered
  5. 5
    기타solvent evaporated in vacuo
  6. 6
    기타The crude product was purified by flash column chromatography (hexanes:ethyl acetate 100:0 to 90:10)

실험 절차

A solution of the product of Example 8B (1.57 g, 14.05 mmoles), imidazole (1.43 g, 21.08 mmoles), and Tert-butyl-chlorodiphenylsilane (4.76 gm, 17.4 mmoles) in N,N-dimethylformamide (10 mL) was stirred for five hours at 23° C. The reaction was partitioned between ethyl acetate and water. The organic layer was washed with brine (25 mL), dried with MgSO4, filtered, and solvent evaporated in vacuo. The crude product was purified by flash column chromatography (hexanes:ethyl acetate 100:0 to 90:10) to provide the title compound as an oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737137B2uspto-grants-2010_06