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morphine from codeine synthesis

hockey34

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will this method work?

A solution of 3.00 grams (10 mmol) of codeine in 60 ml of dry dimethylformamide was degassed under nitrogen by repeatedly stirring under vacuum, followed by inletting nitrogen. Following the addition of 3.00 grams (26.7 mmol) of potassium tert-butoxide, the degassing process was repeated, and 3.0 ml (32.7 mmol) of n-propanethiol was injected by syringe. The mixture was stirred at 125°C under nitrogen for 45 min (similar results at 110°C for 3h), cooled, and quenched with 3.0 ml of acetic acid. The solvent was removed under high vacuum, and the residue dissolved in 30 ml of 1N hydrochloric acid. The acid solution was washed with several portions of ether, treated with 5ml of 20% sodium bisulfite, and alkalized to pH 9 with ammonium hydroxide. The precipitated solid was collected, washed with water, and dried in vacuo (100°C) to leave 2.30g (80%) of morphine as tan crystals.

how and why is the n-propanethiol injected by syringe?
 

hockey34

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can anyone comment on this?
 

hockey34

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can an addition funnel be used instead of a syringe for the addition of n-propanethiol?
 

41Dxflatline

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the point of the syringe is to keep your nitrogen atmosphere intact.
 

hockey34

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the point of the syringe is to keep your nitrogen atmosphere intact.
41Dxflatlinethank you. what kind of flask neck is needed to inject with a syringe? do you need a special bung?

what kind of syringe should be used?
 

41Dxflatline

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thank you. what kind of flask neck is needed to inject with a syringe? do you need a special bung?

what kind of syringe should be used?
hockey34Necks not important, you just need 'rubber septa' that you can seal it with. Syringe doesn't matter as long as its big enough, glass is preferable since it doesn't melt when it touches the wrong solvent
 

hockey34

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Necks not important, you just need 'rubber septa' that you can seal it with. Syringe doesn't matter as long as its big enough, glass is preferable since it doesn't melt when it touches the wrong solvent
41Dxflatlineshouldn't the syringe have a hypodermic needle to penetrate the rubber septa? and should the needle stay in the rubber septa instead of removing it so that none of the gas in the flask escapes through the hole that the needle made?
 
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