1-(4-chlorophenyl)-2,2-dimethylpropan-1-one

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 29.5 g ofg 4-chlorophenyl tert.-butyl ketone (0.15 mol) in 750 ml ethanol was heated under reflux with an excess (118 ml) of methl hydrazine and 3 ml of concentrated sulphuric acid for 4.5 hours. It was concentrated almost to dryness and the added to water. After extraction with methylene chloride and then drying and concentrating the extract in vacuo, there was obtained an oil which eventually crystallised. The resulting crude product used immediately. It was concentrated almost to dryness the added to water After extraction with methylene chloride drying concentrating the extract in vacuo there was obtained an oil which eventually crystallised

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 29.5 g ofg 4-chlorophenyl tert.-butyl ketone (0.15 mol) in 750 ml ethanol was heated under reflux with an excess (118 ml) of methl hydrazine and 3 ml of concentrated sulphuric acid for 4.5 hours. It was concentrated almost to dryness and the added to water. After extraction with methylene chloride and then drying and concentrating the extract in vacuo, there was obtained an oil which eventually crystallised. The resulting crude product used immediately. It was concentrated almost to dryness the added to water After extraction with methylene chloride drying concentrating the extract in vacuo there was obtained an oil which eventually crystallised

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 4.92 g (0.025 mol) 4-chlorphenyl tert.-butyl ketone and 8.05 g (0.075 mol) ethyl carbazate in 125 ml absolute ethanol was treated with ca. 0.3 g concentrated sulphuric acid and heated at reflux for 3 hours. The solution was then concentrated in vacuo and the residue added to water. It was then extracted with ethyl acetate, the organic phase dried with magnesium sulphate, concentrated and the residue recrystallised from diisopropyl ether. heated at reflux for 3 hours The solution was then concentrated in vacuo the residue added to water It was then extracted with ethyl acetate the organic phase dried with magnesium sulphate concentrated the residue recrystallised from diisopropyl ether

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 4.92 g (0.025 mol) 4-chlorphenyl tert.-butyl ketone and 8.05 g (0.075 mol) ethyl carbazate in 125 ml absolute ethanol was treated with ca. 0.3 g concentrated sulphuric acid and heated at reflux for 3 hours. The solution was then concentrated in vacuo and the residue added to water. It was then extracted with ethyl acetate, the organic phase dried with magnesium sulphate, concentrated and the residue recrystallised from diisopropyl ether. heated at reflux for 3 hours The solution was then concentrated in vacuo the residue added to water It was then extracted with ethyl acetate the organic phase dried with magnesium sulphate concentrated the residue recrystallised from diisopropyl ether

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of dimethyl oxosulphonium methylide was prepared under nitrogen from sodium hydride (0.03 mol) and powdered trimethyl oxosulphonium iodide (0.03 mol) in dry dimethyl sulphoxide (40 ml). A solution of 4-chlorophenyl tertiary butyl ketone (0.025 mol) in dry dimethyl sulphoxide (10 ml) was added dropwise at room temperature and the solution heated at 50° C. for 2.5 hours. After cooling to room temperature the solution was extracted with ether (150 ml), washed with water and dried over anhydrous sodium sulphate. Removal of the solvent gave 1-(4-chlorophenyl)-1-t-butyl-ethylene oxide (95%) as a colourless liquid. After cooling to room temperature the solution was extracted with ether (150 ml) washed with water dried over anhydrous sodium sulphate Removal of the solvent

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Trimethyl acetonitrile (0.1 mol) in dry tetrahydrofuran (50 ml) was added dropwise with stirring to the Grignard reagent prepared form 4-chloro-iodobenzene (0.11 mol) and magnesium turnings (0.11 g atoms) in sodium dry ether (50 ml) at such a rate as to retain gentle reflux. The solution was refluxed for 4 hours, cooled to room temperature, and water (40 ml) added carefully. 2N H2SO4 (50 ml) was added and the ether solution washed with water (3×100 ml) and dried over anhydrous magnesium sulphate. Removal of the solvent gave a yellow oil which was distilled at the water pump to give tertiary butyl 4-chlorophenyl ketone (40%) as a colourless liquid b.p. 116°-128°/15 mm Hg. The solution was refluxed for 4 hours the ether solution washed with water (3×100 ml) dried over anhydrous magnesium sulphate Removal of the solvent gave a yellow oil which was distilled at the water pump

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 29.5 g ofg 4-chlorophenyl tert.-butyl ketone (0.15 mol) in 750 ml ethanol was heated under reflux with an excess (118 ml) of methl hydrazine and 3 ml of concentrated sulphuric acid for 4.5 hours. It was concentrated almost to dryness and the added to water. After extraction with methylene chloride and then drying and concentrating the extract in vacuo, there was obtained an oil which eventually crystallised. The resulting crude product used immediately. It was concentrated almost to dryness the added to water After extraction with methylene chloride drying concentrating the extract in vacuo there was obtained an oil which eventually crystallised

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 4.92 g (0.025 mol) 4-chlorphenyl tert.-butyl ketone and 8.05 g (0.075 mol) ethyl carbazate in 125 ml absolute ethanol was treated with ca. 0.3 g concentrated sulphuric acid and heated at reflux for 3 hours. The solution was then concentrated in vacuo and the residue added to water. It was then extracted with ethyl acetate, the organic phase dried with magnesium sulphate, concentrated and the residue recrystallised from diisopropyl ether. heated at reflux for 3 hours The solution was then concentrated in vacuo the residue added to water It was then extracted with ethyl acetate the organic phase dried with magnesium sulphate concentrated the residue recrystallised from diisopropyl ether