반응 #83086

ord-9cf9b2e152cf4134b30a35eb7c1e4df0

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The temperature is maintained below -10° C. during the addition
  2. 2
    여과The reaction is filtered
  3. 3
    농축the filtrate concentrated in vacuo to an oily residue
  4. 4
    기타The residue is purified by chromatography (silica gel: 50% ethyl acetate/hexane)

실험 절차

To a -20° C. solution, under argon, of 8.4 ml of trifluoromethanesulfonic anhydride in 75 ml of methylene chloride is added, dropwise, a solution of 5.9 g of product from Example 268 and 4.05 ml of pyridine in 25 ml of methylene chloride. The temperature is maintained below -10° C. during the addition. The progress of the reaction is monitored by tic. The reaction is filtered and the filtrate concentrated in vacuo to an oily residue, The residue is purified by chromatography (silica gel: 50% ethyl acetate/hexane) to give 7.03 g of the desired product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05623081uspto-grants-1997_04