Reaktion #1561478

ord-beeecb05bd9b46caa3c6e06e27f149f8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvents were removed on a rotary evaporator
  2. 2
    workup.DISSOLUTIONthe residue was redissolved in aq NaHCO3 solution
  3. 3
    ExtraktionThe solution was extracted with IPA-CHCl3 (3:1) twice (50 mL each)
  4. 4
    ExtraktionThe extractions
  5. 5
    Trocknendried over sodium sulfate
  6. 6
    Einengenconcentrated

Vorschrift

To a solution 1,1-dimethylethyl-4-[(4-cyano-5-fluoro-2,3-dihydro-1H-inden-1-yl)methyl]piperazine-1-carboxylate (0.060 g) in DCM (2 mL) was added 4N HCl (2 mL) at RT. The mixture was allowed to stir at RT for 2 hours. The solvents were removed on a rotary evaporator, and the residue was redissolved in aq NaHCO3 solution. The solution was extracted with IPA-CHCl3 (3:1) twice (50 mL each). The extractions were combined, dried over sodium sulfate, and concentrated to give 5-fluoro-1-(piperazin-1-ylmethyl)-2,3-dihydro-1H-indene-4-carbonitrile. LC-MS (IE, m/z): 260 [M+1]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09018211B2uspto-grants-2015_04