The preparation and purification of tritium-labelled hexoestrol of very high specific activity on the 5 mg. scale

Abstract

An apparatus for the catalytic hydrogenation of unsaturated organic compounds on the scale of 50 [mu]moles is described. It is used for the hydrogenation of dienoestrol with hydrogen containing up to 97% of tritium, when a product of specific activity 118 mc/mg. is obtained. A method for the separation of the isomeric products hexoestrol and isohexoestrol on alumina-impregnated paper is given together with a column-partition method for the further purification of the separated hexoestrol from unlabelled impurities derived from the paper. A spectrophotometric method for the detection of unchanged dienoestrol in the reduction products to a lower limit of 2% is also described. Hydrogen uptake usually ceases within a few hours, when it is found that the theoretical volume of hydrogen ([plus or minus] 2%) has been taken up and less than 2% of unchanged dienoestrol remains in the reaction mixture.