ジラール試薬Pを用いる6-オキソエストラジオールの単離精製法

概要

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An efficient synthetic method of 6-oxoestradiol was established by modifying the previous method by Garza and Rao. The present method is characterized by the quantitative extraction of 6-oxoestradiol produced during an oxidation reaction using Girard's reagent P (GP). The procedure is as follows : (1) reaction of estradiol-3,17-diacetate with 5-dimethylpyrazole/chromium trioxide complex in dichloromethane ; (2) column chromatography (SiO_2) of the reaction mixture to obtain steroidal fraction by dichloromethane as an eluent, followed by saponification of the eluate ; (3) reaction of the product with GP in methanol ; (4) removal of the nonketonic steroid from an aq. layer, where the hydrazone of 6-oxoestradiol is remained ; (5) formation of 6-oxoestradiol by acidification of the aq. layer. The overall yield of the 6-oxoestradiol from estradiol was greater than 45 percent.
社団法人日本分析化学会の論文
1997-11-05