Внимательно прочитав предыдущую статью , прикинув в уме Простоту и Изящество синтеза, а так же его финансовую подоплёку , пытливый естествоиспытатель конечно же задастся вопросом , а где взять Фенилацетальдегид ? Отвечу .
Проще всего брать его из банки !
Но ежели по трагическому стечению обстоятельств данная банка была утрачена , в вихре повседневных забот , трудов и развлечений ТО !!! Вот она , методика )
, Phenylacetaldehyde.41 An alkaline solution of sodium hypochlorite isprepared by passing 55 g. of chlorine into a mixture of 600 g. of crackedice and a cold solution of 100 g. of sodium hydroxide (95%) in 150 cc. ofwater. Water is then added until the total volume of the^solution is 11.(The solution is best kept in the dark until used.) To a solution of 14.7 g.(0.1 mole) of cinnamic amide (m.p. 147°) in 125 cc. of methanol is added130 cc. of the stock solution of sodium hypochlorite. The mixture iswarmed on the water bath. A thick sludge of crystals soon forms. Themixture is cooled rapidly and filtered, and the crystals are washed withdilute ethanol and with water. The yield of methyl styrylcarbamate soobtained is 13 g. (70%), m.p. 117-118°.Twenty-five grams of the urethan is dissolved in 100 cc. of warmethanol, and to the solution is added gradually 48 cc. of 6 N sulfuric acid.Carbon dioxide is evolved, and some urethan precipitates, but redissolves quickly when the solution is warmed. When all the sulfuric acidhas been added, the aldehyde is distilled at once with steam. Theproduct so obtained is a colorless oil, b.p. 9O-92°/20 mm. The yield isgood.
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Вот собственно оригинал статьи
Проще всего брать его из банки !
Но ежели по трагическому стечению обстоятельств данная банка была утрачена , в вихре повседневных забот , трудов и развлечений ТО !!! Вот она , методика )
, Phenylacetaldehyde.41 An alkaline solution of sodium hypochlorite isprepared by passing 55 g. of chlorine into a mixture of 600 g. of crackedice and a cold solution of 100 g. of sodium hydroxide (95%) in 150 cc. ofwater. Water is then added until the total volume of the^solution is 11.(The solution is best kept in the dark until used.) To a solution of 14.7 g.(0.1 mole) of cinnamic amide (m.p. 147°) in 125 cc. of methanol is added130 cc. of the stock solution of sodium hypochlorite. The mixture iswarmed on the water bath. A thick sludge of crystals soon forms. Themixture is cooled rapidly and filtered, and the crystals are washed withdilute ethanol and with water. The yield of methyl styrylcarbamate soobtained is 13 g. (70%), m.p. 117-118°.Twenty-five grams of the urethan is dissolved in 100 cc. of warmethanol, and to the solution is added gradually 48 cc. of 6 N sulfuric acid.Carbon dioxide is evolved, and some urethan precipitates, but redissolves quickly when the solution is warmed. When all the sulfuric acidhas been added, the aldehyde is distilled at once with steam. Theproduct so obtained is a colorless oil, b.p. 9O-92°/20 mm. The yield isgood.
ВСЕ БУДЕТ ИСГУД )))
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