反应 #7413

ord-993085dca3ef4537b2715ac868b3332c

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤the resultant solution washed with saturated sodium bicarbonate (1 ml) in a hydrophobic frit
  2. 2
    浓缩The solvent was concentrated under reduced pressure
  3. 3
    其他the residue purified by mass

实验过程

To a solution of acetaldehyde (0.041 ml from a stock solution made up from 0.0127 l acetaldehyde dissolved in 1 ml DCM)) in dry DCM (0.4 ml) treated with acetic acid (0.1 ml from a stock solution made up from 0.0054 ml acetic acid dissolved in 1 ml DCM) was added N-{(3S)-1-[(1S)-2-(3-aminopiperidin-1-yl)-1-methyl-2-oxoethyl]-2-oxopyrrolidin-3-yl }-6-chloronaphthalene-2-sulfonamide [Example 365] (0.045 g) followed by tetraethylammonium triacetoxyborohydride (0.005 g). The mixture was stirred at room temperature, under nitrogen, for 60 h. DCM (1 ml) was added and the resultant solution washed with saturated sodium bicarbonate (1 ml) in a hydrophobic frit. The solvent was concentrated under reduced pressure and the residue purified by mass directed preparative h.p.l.c. to give the title compound (0.8 mg) as an oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07084139B2uspto-grants-2006_08