Reaktion #490006

Reaktionsgleichung

methyl 4-(2-oxo-1-oxa-3,8-diazaspiro[4.5]dec-3-yl)benzoate hydrochloride salt

1-bromo-5-(bromomethyl)-2,3-dichlorobenzene

DIPEA

→

title compound

Ausbeute 94.0%

methyl 4-[8-(3-bromo-4,5-dichlorobenzyl)-2-oxo-1-oxa-3,8-diazaspiro[4.5]dec-3-yl]benzoate

Ausbeute 94.0%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe mixture was evaporated
2. 2
   workup.DISSOLUTIONthe residue was dissolved in saturated aqueous NaHCO3
3. 3
   Extraktionextracted with DCM
4. 4
   SonstigeThe organic layer was evaporated

Vorschrift

To methyl 4-(2-oxo-1-oxa-3,8-diazaspiro[4.5]dec-3-yl)benzoate hydrochloride salt (50 mg, 0.153 mmol; Example 1, Step 2) and 1-bromo-5-(bromomethyl)-2,3-dichlorobenzene (53.7 mg, 0.168 mmol; from Patent US2007/070805) was added DMF (1.5 mL) and DIPEA (107 μL, 0.612 mmol). The mixture was heated to 55° C. for 2 hours. The mixture was evaporated and the residue was dissolved in saturated aqueous NaHCO3 and then extracted with DCM. The organic layer was evaporated to provide the title compound as a yellow oil (76 mg) that was used without further purification.

Quelle