반응 #347375

ord-9c0d00efe18f4cb6b745fe1303d9bee6

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere gradually added to the mixture
  2. 2
    추출extracted twice
  3. 3
    추출The combined extract
  4. 4
    세척was washed with water
  5. 5
    건조dried over anhydrous Na2SO4
  6. 6
    workup.DISTILLATIONdistilled on rotovap
  7. 7
    기타Yield

실험 절차

To an ice cold solution of 1.15 g (3 mmol) of the product of Example 27 in 200 ml of deaerated water, 1.5 g (18 mmol) sodium bicarbonate were added. While the mixture was bubbled with N2 gas, 2.09 g (12 mmol) of sodium dithionite were gradually added to the mixture. The mixture was stirred under N2 for 1 hr and then extracted twice, each with 100 ml of ethyl acetate. The combined extract was washed with water, dried over anhydrous Na2SO4 and distilled on rotovap. Yield, 0.38 g (50%) of yellowish semisolid which reduced alcoholic AgNO3TS instantaneously. (PMR as expected.)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05525727uspto-grants-1996_06