反応 #631034

反応方程式

(11β)-2,2'-[(9-fluoro-11-hydroxy-3-oxoandrosta-1,4-dien-17,17-diyl)bis(thio)]bisacetic acid, diethyl ester

→

title compound

収率 82.3%

(11β)-[(9-Fluoro-11-hydroxy-3-oxoandrosta-1,4,16-trien-17-yl)thio]acetic acid, ethyl ester

収率 82.3%

溶媒

diethylbenzene

chloroform

反応条件

後処理

1. 1
   温度The solution was then cooled
2. 2
   workup.ADDITIONwas poured on a column of silica gel (60 g)
3. 3
   洗浄eluting the column successively with chloroform and chloroform-ethyl acetate (95:5, 9:1 and 4:1)

実験手順

A solution of (11β)-2,2'-[(9-fluoro-11-hydroxy-3-oxoandrosta-1,4-dien-17,17-diyl)bis(thio)]bisacetic acid, diethyl ester (6.48 g; see example 2) in dry diethylbenzene (200 ml) was refluxed in contact with air for 4.0 hours. The solution was then cooled, diluted with some chloroform and was poured on a column of silica gel (60 g), eluting the column successively with chloroform and chloroform-ethyl acetate (95:5, 9:1 and 4:1) to isolate the title compound (4.15 g). One crystallization of this from ethyl acetate-hexane gave the analytical specimen of the title compound (3.8 g), melting point 144°-145° C., with consistent spectral data.

出典