تفاعل #792141
ord-855ed5f194584302be2c3940b738ae72
معادلة التفاعل
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1درجة الحرارةat reflux
- 2workup.STIRRINGthe reaction mixture is further stirred for 2 hrs
- 3درجة الحرارةat reflux
- 4أخرىThe cooled reaction mixture
- 5ترشيحis then filtered over a cake of diatomaceous earth
- 6غسيلThe cake is washed twice by 80 ml of methanol
- 7تركيزthe combined methanolic extracts are concentrated under vacuum
- 8workup.ADDITION100 ml of water are then added to the residue
- 9استخلاصThe watery layer is extracted with 300 ml of ethyl acetate
- 10غسيلThe organic layer is washed twice by brine
- 11ترشيحfiltered over a phase separator paper
- 12أخرىto yield after concentration 5 g of a yellow oil
الإجراء التجريبي
To a cooled solution of 3.5 g (21.8 mmol) of 1-(indan-2-yl)ethanone in 100 ml of methanol, are added 10 g of 3 Å molecular sieves and 2.3 g (40.2 mmol) of cyclopropylamine followed by a slow addition of 2.87 ml (50.2 mmol) of acetic acid. The reaction mixture is stirred for 2.5 hrs at reflux. The reaction mixture is then cooled to 0° C. and 1.9 g (30 mmol) of sodium cyanoborohydride are slowly added and the reaction mixture is further stirred for 2 hrs at reflux. The cooled reaction mixture is then filtered over a cake of diatomaceous earth. The cake is washed twice by 80 ml of methanol and the combined methanolic extracts are concentrated under vacuum. 100 ml of water are then added to the residue and the pH is ajusted to 12 with a 0.5 N solution of sodium hydroxyde. The watery layer is extracted with 300 ml of ethyl acetate. The organic layer is washed twice by brine and filtered over a phase separator paper to yield after concentration 5 g of a yellow oil. Column chromatography on silica gel (gradient heptane/ethyl acetate) yields 1.2 g (28% yield) of N-[1-(indan-2-yl)ethyl]cyclopropanamine as a colourless oil (M+H =202).