Process for the preparation of .beta.-methyldigoxin
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United States of America Patent
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Jul 29, 1986
Issued Date -
N/A
app pub date -
May 21, 1984
filing date -
Apr 27, 1983
priority date (Note) -
Expired
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Abstract
The invention relates to a process for the preparation of .beta.-methyldigoxin by the selective methylation of digoxin with dimethyl sulfate in the presence of a basic strontium compound and, if appropriate, of an inert inorganic adsorbent. Strontium hydroxide octahydrate, strontium methylate or strontium hydroxymethylate is used as the basic strontium compound, and an oxide, silicate or phosphate of magnesium, calcium, aluminum, silicon or titanium, with a water content in the range of 0 to 20% by weight, is used as the inorganic adsorbent. The reaction is carried out at temperatures of -15.degree. to 15.degree. C. in the presence of 3 to 24 moles of water per mole of digoxin, the water being introduced in the reaction mixture by the water content of strontium hydroxide octahydrate and/or the inorganic adsorbent used and purification of the methylation product so formed by column chromatography on SiO.sub.2 with a mixture of chlorohydrocarbon and a lower aliphatic alcohol.
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