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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 2065998Erstellt: 27. Oktober 2026

Methanol → Exemestane

https://huagongshe.com/reaction/2065998

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktMethanolHCID 887—
EduktChloranilHCID 8371—
Edukttert-Butyl methyl etherHCID 15413—
Edukt6-Methylideneandrost-4-ene-3,17-dioneHCID 12951800—
Lösungsmittel1-MethylpyrrolidineHCID 8454—
ProduktExemestaneHCID 6019860,4%

Reaktionsbedingungen

Temperatur77.5 °C

Reaktionsschritte

6-Methylen-androst-4-ene-3,17-dione (5.0 gm) was dissolved in N-methylpyrrolidine (25 mL) at RT & to it was charged Chloranil (12.37 gm) at RT. The reaction mass was heated to 75 to 80° C. for 18 hours. The progress of the reaction is monitored on TLC. The reaction mass was cooled down to room temperature and methanol was added to it. The reaction mass was stirred for next 30 minutes and precipitated solid mass was filtered through buchner funnel and washed with methanol. All the filtrates were combined and suitably diluted. The product from aqueous solution was extracted in toluene. Combined toluene extracts was washed with 2% aqueous NaOH solution under stirring for 30 minutes. The toluene layer was separated and washed with water. Toluene layer was dried over sodium sulfate, filtered and evaporated at reduced pressure to get solid residue. The solid residue was treated with MTBE to get 3.0 gm solid product. HPLC Purity: 97%.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08288571B2
Quelldatensatzuspto-grants-2012_10
ORD IDord-8871462b30404e98ae28401dc193bab5
Quellennotizuspto-grants-2012_10