Reaktion #714101

Reaktionsgleichung

tert-Butyl (2S,5S)-2-[4-methyl-6-[4-(trifluoromethyl)phenyl]pyrimidin-2-yl]-6-oxo-1,7-diazaspiro[4.4]nonane-1-carboxylate

HCl

1,4-dioxan

→

(2S,5S)-2-[4-methyl-6-[4-(trifluoromethyl)phenyl]pyrimidin-2-yl]-1,7-diazaspiro[4.4]nonan-6-one

NH3 MeOH

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solution was evaporated
2. 2
   Sonstigere-evaporated with toluene (25 ml)
3. 3
   workup.DISSOLUTIONThe residue was dissolved in MeOH (2 ml)
4. 4
   Wascheneluting with MeOH

Vorschrift

tert-Butyl (2S,5S)-2-[4-methyl-6-[4-(trifluoromethyl)phenyl]pyrimidin-2-yl]-6-oxo-1,7-diazaspiro[4.4]nonane-1-carboxylate (37 mg, 0.0800 mmol) was added to a stirred solution of 4M HCl in 1,4-dioxan (2 mL, 8 mmol) in DCM (2 mL) at ambient temperature. The colourless solution was stirred in a stoppered flask for 4 h. The solution was evaporated and re-evaporated with toluene (25 ml). The residue was dissolved in MeOH (2 ml) and passed through a 2 g SCX cartridge, eluting with MeOH then 1M NH3-MeOH to give (2S,5S)-2-[4-methyl-6-[4-(trifluoromethyl)phenyl]pyrimidin-2-yl]-1,7-diazaspiro[4.4]nonan-6-one (31 mg);

Quelle