1-morpholin-4-ylpropan-2-one

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

実験手順: The title compound was prepared from 1-morpholinopropan-2-one (4.192 g, 29.3 mmol), Sodium (0.43 g, 29.3 mmol), diethyl oxalate (4.28 g, 29.3 mmol) and hydrazine hydrochloride (2 g, 29.3 mmol) using the method of Example 225(a). Yield 18%. 1H NMR (400 MHz; CDCl3): δ 1.39 (t, 3H), 2.48 (m, 4H), 3.60 (d, 2H), 3.71 (m, 4H), 4.38 (q, 2H), 6.74 (s, 1H).

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of N-(2-oxopropyl)morpholine (82 g, 0.57 mmol) in diethyl ether (400 ml) was added to a solution of 3M CH3MgBr (500 ml, 1.5 ml) in anhydrous diethyl ether (21) and stirred at 0° C. under an argon atmosphere. The mixture was stirred at ambient temperature for 16 hours, treated with 12N HCl (50 ml) and extracted with ethyl acetate. The product was purified by flash column chromatography eluting with ethyl acetate to give N-(2-hydroxy-2-methylpropyl)morpholine. The mixture was stirred at ambient temperature for 16 hours extracted with ethyl acetate The product was purified by flash column chromatography eluting with ethyl acetate

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

実験手順: 15 g of piperonal (0.1 mole), and 14.3 g of 3-morpholinoacetone (0.1 mole) are mixed in an aqueous-alcoholic sodium hydroxide solution (300 cm3 of 10% NaOH and 30 cm3 of ethanol). The mixture is stirred for 4 hours and the product obtained is then filtered. The product is rinsed with water and recrystallised from ethanol. the product obtained is then filtered The product is rinsed with water recrystallised from ethanol

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

実験手順: Condensation 13.6 g (0.1 mole) of p-methoxybenzaldehyde is dissolved in 14.3 g (0.1 mole) of morpholinoacetone and this solution is added dropwise to 100 cm3 of a solution of 1 N sodium hydroxide cooled in an ice-containing water bath. The temperature is allowed to return to ambient temperature while stirring for 5 hours. The precipitate obtained is filtered and rinsed several times with water. 18.8 g of 1-(p-methoxyphenyl)-4-morpholino-1-buten-3-one is obtained. containing water bath to return to ambient temperature The precipitate obtained is filtered rinsed several times with water

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

実験手順: The title compound was prepared from 1-morpholinopropan-2-one (4.192 g, 29.3 mmol), Sodium (0.43 g, 29.3 mmol), diethyl oxalate (4.28 g, 29.3 mmol) and hydrazine hydrochloride (2 g, 29.3 mmol) using the method of Example 225(a). Yield 18%. 1H NMR (400 MHz; CDCl3): δ 1.39 (t, 3H), 2.48 (m, 4H), 3.60 (d, 2H), 3.71 (m, 4H), 4.38 (q, 2H), 6.74 (s, 1H).