- Carprost tromethamine related impurity levobutyl 15-ketone and preparation method thereof
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The invention relates to the technical field of compounds and preparation thereof, in particular to a prostaglandin tromethamine related impurity levobutyl 15-ketone and a preparation method thereof.The method comprises the following steps that 1, in the presence of a fifth organic solvent, strong base is used for carrying out dehydrogenation reaction on methyl triphenyl phosphine halide, ethyl butyrate is added after the reaction is carried out for a certain period of time, and a reaction solution is obtained; continuously reacting for a certain time to obtain 1-triphenylphosphine- 2-pentanone; and (2) carrying out wittig reaction on the 1-triphenylphosphine- 2-pentanone obtained in the step (1) and a second organic solvent solution of benzoyl corey lactone aldehyde to obtain butyl-15 ketone. The method has the characteristics that the operation is simple and convenient, the safety is high, the yield and the purity of the obtained product are high under optimal conditions, the requirements for impurity research can be met, and the like.
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Paragraph 0029; 0034-0035; 0037-0038
(2021/01/15)
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- Highly substituted tetrahydropyrones from hetero-Diels-Alder reactions of 2-alkenals with stereochemical induction from chiral dienes
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(Chemical Equation Presented) A new method for the stereoselective synthesis of libraries of 2,3,5-trisubstituted tetrahydro-γ-pyrones and the corresponding tetrahydropyran-4-ols is reported. Dienes with a chiral moiety at position 5 were synthesized star
- Ruijter, Eelco,Schueltingkemper, Heike,Wessjohann, Ludger A.
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p. 2820 - 2823
(2007/10/03)
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- Antitumour polycyclic acridines. Part 13. Synthesis of 2-substituted 7H-pyrido[4,3,2-kl]acridines by thermolysis of 9-(5-alkyltriazol-1-yl)acridines
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Interaction of phosphoranylidene ketones with 9-azidoacridine in refluxing benzene affords 9-(5-substituted triazol-1-yl)acridines, which, on thermolysis in boiling diphenyl ether at 259 °C, yield 2-substituted 7H-pyrido[4,3,2-kl] acridines in high yields. These tetracyclic acridines are less potent inhibitors of human tumour cells in vitro than their pentacyclic analogues.
- Ellis, Michael J.,Stevens, Malcolm F. G.
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- Flash Vacuum Pyrolysis of Stabilised Phosphorus Ylides. Part 1. Preparation of Aliphatic and Therminal Alkynes
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Thermal extrusion of Ph3PO from β-oxoalkylidenetriphenylphosphoranes 4 to give the alkynes 5, which under conventional pyrolysis conditions is restricted to cases in which R1 is an electron withdrawing group, has been successfully achieved for R1=H or alkyl by using FVP.The method allows convenient construction of multigram quantities of the alkynes 5 from alkyl halides 1 and allows convenient construction of multigram quantities of the alkynes 5 from alkyl halides 1 and acid chlorides 3 in three steps with good overall yields.Under the conditions used the ylides with R2 = cyclobutyl also undergo less of ethene to provide convenient access to the vinylalkynes 6.
- Aitken, R. Alan,Atherton, J. Ian
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p. 1281 - 1284
(2007/10/02)
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- Synthesis and reactions of [1-(trialkylsilyl)alkylidene]triphenylphosphoranes
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Alkylidenetriphenylphosphoranes 1 react with trialkyl halosilanes 2 to afford silylated alkylidenephosphoranes 5, which can be converted to acylated alkylidenephosphoranes 8 and 10 by trimethylsilyl carboxylates 6 or carboxylic anhydrides 10. Bis(acylalkylidenephosphoranes) 13-15 are available from 5 and bis(trimethylsilyl) dicarboxylates 12 or cyclic or polymeric anhydrides 16, 17.
- Bestmann,Bomhard,Dostalek,Pichl,Riemer,Zimmermann
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p. 787 - 792
(2007/10/02)
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- Cumulated Ylides, XVI. A Method for the Exchange of the OH Group in Free Carboxylic Acids by the Ylide Function
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Carboxylic acids 5 react with triphenylphosphorane (4) via the intermediate 6 with formation of the phosphoranes 7, which rearrange by heating in an intramolecular acyl migration to ylides 10.By heating of 10 in the presence of an alcohol 13 the acyl ylides 11 and urethanes 14 are formed.The reaction sequence allows the replacement of the OH group in carboxylic acids by the ylide function.
- Bestmann, Hans Juergen,Schade, Gerold,Schmid, Guenter,Moenius, Thomas
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p. 2635 - 2639
(2007/10/02)
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- Cyclopentanone derivatives
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Cyclopentane derivatives of the formula: STR1 wherein R1 represents hydrogen or a carboxylic acyl group, and either (I) R2 represents a group of the formula: (wherein R3 and R4 represent hydrogen or alkyl, and R5 represents hydrogen, or alkyl, alkoxy, cycloalkyl or adamantyl, or R5 represents alkyl substituted by alkoxy, or by cycloalkyl or by adamantyl, or the group --CR3 R4 R5 together forms a cycloalkyl or adamantyl group), X represents trans-vinylene or ethylene and Y represents carbonyl or a group of the formula: STR2 wherein R6 represents hydrogen or alkyl, and R7 represents hydrogen or a carboxylic acyl group, or else (ii) R2 represents a group of the formula: (wherein A represents alkylene, Z represents a direct bond or oxygen or sulphur, and R8 represents an aryl or heterocyclyl group which may be substituted by one or more of halogen, alkyl, alkoxy and trihalomethyl), X in formula I represents ethylene or trans-vinylene and Y in formula I represents carbonyl or a group of formula III, or else (iii) R2 represents a group R8 and X and Y in formula I represent simultaneously ethylene and carbonyl, trans-vinylene and carbonyl, or ethylene and --CH(OR7)-- groups respectively. The compounds are new and possess pharmacological properties similar to those of prostaglandins.
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