反応 #702181

反応方程式

17,17-bis(ethylthio)-9-fluoro-11β-hydroxyandrosta-1,4-dien-3-one

→

tlc-homogeneous material

収率 87.9%

17-(Ethylthio)-9-fluoro-11β-hydroxyandrosta-1,4,16-trien-3-one

収率 87.9%

溶媒

diethylbenzene

反応条件

後処理

1. 1
   温度The solution is cooled to 0° C.
2. 2
   その他the solid that precipitates
3. 3
   ろ過is filtered
4. 4
   workup.DISSOLUTIONThis is redissolved in 1:9 hexane-chloroform
5. 5
   その他chromatographed on a 60 g-silica gel column
6. 6
   洗浄Elution with 1:9 hexane-chloroform

実験手順

A suspension of 1.8 g of 17,17-bis(ethylthio)-9-fluoro-11β-hydroxyandrosta-1,4-dien-3-one in 120 ml of diethylbenzene is stirred at 190° C. (oil bath temperature) for 1 hour. The solution is cooled to 0° C. and the solid that precipitates is filtered. This is redissolved in 1:9 hexane-chloroform and chromatographed on a 60 g-silica gel column. Elution with 1:9 hexane-chloroform gives 1.35 g of a tlc-homogeneous material. Crystallization from chloroform-methanol gives 680 mg of the title compound, melting point 282°-283° C., dec.

出典