반응 #159490

ord-5f047d3589634eab8b0854184cd30d04

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The cooling was removed
  2. 2
    기타reaction mixture
  3. 3
    workup.STIRRINGwas stirred at room temperature under N2 for 24 h
  4. 4
    추출the mixture extracted by EtOAc
  5. 5
    세척The combined organic layer was washed by H2O
  6. 6
    건조brine, and dried over MgSO4
  7. 7
    기타The solvent was evaporated
  8. 8
    기타the obtained oil was dried overnight in high vacuum

실험 절차

To a solution of Boc-Ser-OH (0.3 g, 1.46 mmol, 1 eq) in dry DMF (4 ml) at 0° C., dry K2CO3 (0.22 g, 1.6 mmol, 1.1 eq) was added. The resulting white suspension was stirred for 15 minute and ethyl iodide (0.68 g, 0.35 ml, 4.38 mmol, 3 eq) was dropwise added. The cooling was removed and reaction mixture was stirred at room temperature under N2 for 24 h. To the formed white emulsion H2O was added, and the mixture extracted by EtOAc. The combined organic layer was washed by H2O and then brine, and dried over MgSO4. The solvent was evaporated and the obtained oil was dried overnight in high vacuum. Yield of the pure F—0.27 g (79%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08828993B2uspto-grants-2014_09