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home sign in 0 publishing chemspider education community news more... about us advertise with us careers service the chemistry centre (venue hire) chemistry world jobs chemistry world magazine chemnet student networking chemspider synthetic pages conferences & events diversity educational resources library and information centre online shop prizes & awards submission system (journals) talk chemistry ');//-- about about editors advertising search text search structure search browse most accessed recent submissions help searching registering submitting faq text search structure search search by reaction name, author name, or compound why use chemspider syntheticpages? it’s free: no licence or subscription required save time: find a reliable procedure that has already been optimised unique information: discover additional details direct from the researcher e.g. trouble-shooting tips, frequently encountered problems and scale up details why submit a procedure or method? quick and easy: it’s fast and simple to submit. detailed instructions are here . recognition: all published procedures receive a doi making them citable, discoverable and searchable. increase your visibility: submit procedures you have carried out, whether new or well-known, published or unpublished. example reactions biginelli reaction ; n,n'-(4,4'-oxybis(4,1-phenylene))bis(6-methyl-4-phenyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxamide) sirin gülten loading... procedure: a mixture of 3-oxo-n-[4-[4-(-3oxobutanoylamino) phenoxy]phenyl]butanamide (300 mg, 0.814 mmol), thiourea (185 mg, 2.44 mmol), benzaldehyde (0.25 ml, 2.44 mmol) and catalytic amoun of conc. hcl (4 drops) in etoh (10 ml) was refluxed overnight. after the completion of reaction, the reaction mixture was allowed to cool. the solid product formed was filtered, washed with water (5 ml) and cold ether (3x5 ml) to remove the unreacted thiourea or benzaldehyde or 3-oxo-n-[4-[4-(-3oxobutanoylamino) phenoxy]phenyl]butanamide and dried. the title compound was obtained as a light yellow solid (486 mg, 94% yield). methanesulfonylation of phthalic anhydride protected phenylglycinol ; ( r )-2-(1,3-dioxoisoindolin-2-yl)-2-phenylethyl methanesulfonate nikola p. chmel, pratik gurnani loading... procedure: methanesulfonyl chloride (0.32 ml, 4.12 mmol) and tea (0.57 ml, 4.12 mmol) were added to a solution of (r)-2-(2-hydroxy-1-phenylethyl)isoindoline-1,3-dione (1.0 g, 3.7 mmol) in dcm (20 ml) and were stirred overnight. the resulting solution was washed with water (3 × 20 ml) and dried over anhydrous sodium sulphate. the solvents were removed under reduced pressure and the residue was used in the subsequent reaction without further purification. yield 1.22 g (94%). oxidation of a thiol to a sulfonyl chloride ; dodecane-1-sulfonyl chloride nenad maraš loading... procedure: to a stirring solution of dodecane-1-thiol (1.74 g, 86 mmol) in a mixture of acetonitrile and water (4 : 1 vol., 40 ml) on an ice-bath was added portion-wise trichloroisocyanuric acid (2.90 g, 125 mmol) at such a rate to maintain the temperature at no more than 5 °c. the mixture was left stirring for 30 min in the ice-bath. the precipitated cyanuric acid was then removed by filtration and washed with ethyl acetate (30 ml). the combined filtrate was evaporated under reduced pressure at the bath temperature not higher than 30 °c (to minimize the losses from hydrolysis). the so obtained crude product was dissolved in petroleum ether (50 ml), washed with cold 1% hcl(aq) (50 ml), dried over na 2 so 4 and again evaporated under reduced pressure to give the product as a white powder (1.40 g, 61%). advertisement spotlight advertisement about us working for us press office terms of use privacy & cookies accessibility help contact © royal society of chemistry 2018 registered charity number: 207890

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