反応 #83086

ord-9cf9b2e152cf4134b30a35eb7c1e4df0

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05623081uspto-grants-1997_04