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Red (e) -2 - Amino -1 - Chloro-phenyl-propanol Hydrochloride Synthesis And Split

Posted on:2003-12-29Degree:MasterType:Thesis
Country:ChinaCandidate:Y D ZhaoFull Text:PDF
GTID:2191360062475876Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
In this paper, preparation of erythro-2-amino-1-(4-chlorophenyl)-proprane-1-ol from p-chlorphenylpropiophenone and butyl nitrite by oximation, hydrogenation with platinum catalysts and reduction with potassium borohydride was reported. It was showed that the yield was above 40%. A lot of experiments and some improvements were made. In study, we used petroleum ether as the solvent instead of aether during oximation process, which increased the yield above 85% dramatically. The hydrogenation could be carried out by using 2% Pt/C catalyst and methanol as solvent under room temp for 7 hours. The yield of this reaction was 78%. Potassium borohydride which is found to be effective for reduction replaces sodium borohydride as a reducer. The reduction of ketone is carried out under 0癈 for 2 hours using water as solvent The yield of reduction is 83%. After the reduction, we regulated the PH, used methanol to extract the salt. By means of condensation and crystallization, very good crystals could be obtained. By comparison with the original document, many improvements were made on technology, production cost, operation and so on.We also study resolution of erythro-2-amino-1- C 4-chlorophenyl ) -proprane-1-ol.
Keywords/Search Tags:platinum catalysts, potassium borohydride p-chlorphenylpropiophenone, oximation, hydrogenation, erythro-2-amino-1-(4-chlorophenyl)-propane-1-ol
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