Reaktion #86840

ord-0b3eba3b788d4dc386e4666521b0ea7b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas irradiated in a microwave oven for 3 minutes at 100° C
  2. 2
    EinengenThe mixture was concentrated under reduced pressure
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in a solution of sodium hydroxide 6N
  4. 4
    Waschenwashed with dichloromethane
  5. 5
    Extraktionextracted with ethyl acetate
  6. 6
    Sonstigedried
  7. 7
    Einengenconcentrated 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434722B2uspto-grants-2016_09