تفاعل #346336

معادلة التفاعل

11β-trimethylsiloxy-21-acetoxy-6α-fluoropregna-4,16-diene-3,20-dione

→

compound 13

11β-trimethylsiloxy-21-acetoxy-6α-fluoropregna-1,4,16-triene-3,20-dione

المذيبات

dioxan

ظروف التفاعل

المعالجة

1. 1
   أخرىobtained
2. 2
   درجة الحرارةwas heated
3. 3
   درجة الحرارةunder reflux for 2 hours
4. 4
   درجة الحرارةThe resulting dark colored suspension was cooled
5. 5
   ترشيحfiltered from dichloro-dicyanohydroquinone
6. 6
   أخرىevaporated to dryness
7. 7
   workup.DISSOLUTIONThe residue was dissolved in chloroform
8. 8
   أخرىThe solvent was evaporated under reduced pressure
9. 9
   أخرىThe residue was crystallized from methanol

الإجراء التجريبي

A mixture of 3.5 g of 11β-trimethylsiloxy-21-acetoxy-6α-fluoropregna-4,16-diene-3,20-dione obtained according to Example 6, 2.65 g of 2,3-dichloro-4,5-dicyanobenzoquinone (DDQ) and 30 ml of dioxan was heated under reflux for 2 hours. The resulting dark colored suspension was cooled, filtered from dichloro-dicyanohydroquinone, and evaporated to dryness. The residue was dissolved in chloroform and passed through a short column of neutral alumina (50 g). The solvent was evaporated under reduced pressure. The residue was crystallized from methanol. The analytical sample of 11β-trimethylsiloxy-21-acetoxy-6α-fluoropregna-1,4,16-triene-3,20-dione (compound 13) was obtained by an additional recrystallization from methanol. The yield was 2.65 g.

المصدر