Reaktion #86840
ord-0b3eba3b788d4dc386e4666521b0ea7b
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigewas irradiated in a microwave oven for 3 minutes at 100° C
- 2EinengenThe mixture was concentrated under reduced pressure
- 3workup.DISSOLUTIONthe residue was dissolved in a solution of sodium hydroxide 6N
- 4Waschenwashed with dichloromethane
- 5Extraktionextracted with ethyl acetate
- 6Sonstigedried
- 7Einengenconcentrated under reduced pressure
Vorschrift
A mixture of 6,6-dimethyl-5,7-dioxaspiro[2.5]octane-4,8-dione (0.500 g; 2.94 mmol) and 4-isopropylaniline (1.21 mL; 8.82 mmol) in ethanol (3 mL) was irradiated in a microwave oven for 3 minutes at 100° C. The mixture was concentrated under reduced pressure and the residue was dissolved in a solution of sodium hydroxide 6N, washed with dichloromethane, acidified with a solution of hydrochloric acid 6N to pH=2, extracted with ethyl acetate dried and concentrated under reduced pressure to yield 0.036 g (5%) of a pale green solid, which was used in the next step without further purification.