반응 #50038

ord-8f1e1fc265ee4e8686e00515ef1a9f73

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITat ambient temperature for 16 hr
  2. 2
    workup.ADDITIONmixed well
  3. 3
    기타The layers were separated
  4. 4
    추출the aqueous portion was extracted with ether (500 mL)
  5. 5
    세척The combined organic layers were washed with brine (500 mL)
  6. 6
    건조dried (Na2SO4)
  7. 7
    여과filtered
  8. 8
    기타The solvents were evaporated in vacuo

실험 절차

To Carbobenzyloxy-L-proline (Aldrich, 9.80 g, 39.3 mmol) in THF (100 mL) at 0° C. was added BH3 -THF complex (Aldrich, 1M in THF, 100 mL, 100 mmol). The mixture was stirred at 0° C. for 2 hours, then at ambient temperature for 16 hr. The reaction mixture was poured into pH 7 phosphate buffer solution (500 mL) and ether (600 mL) and mixed well. The layers were separated and the aqueous portion was extracted with ether (500 mL). The combined organic layers were washed with brine (500 mL), dried (Na2SO4) and filtered. The solvents were evaporated in vacuo leaving the crude carbobenzyloxy-L-prolinol as an oil (10.5 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05424444uspto-grants-1995_06