- Joined
- Dec 30, 2022
- Messages
- 9
- Reaction score
- 5
- Points
- 3
P2np to p2p
Add to a 500ml Round bottomed boiling flask (RBF) with 3 necks
central neck has an overhead stirrer - IMPORTANT has to be an overhead stirrer and has to be powerful enough to keep iron powder from settling on the bottom, cannot use magnetic stirring as it does not have enough power to keep the iron powder up in the solution and the iron messes with the magnetic stirring anyway.
side neck has a long reflux condenser with cold water supplied
2nd side neck has a pressure-equalising addition funnel filled with 0.197 mole of conc. hydrochloric acid 35.5% in the below example thats is 20.2 ml
The RBF is in a water or oil bath to keep internal reaction temperature at 85 to 95 degC.
Add to RBF:
0.1 mole of P2NP (P2NP 163.2 g/mole) = 16.23g of P2NP
0.715 mole of iron (Fe 55.85 g/mole) = 40g of iron (Fe) - cast iron turnings or ideally 40 mesh iron powder (powder 0.4 mm size)
Note: Activate a metal normally involves rinsing it with a strong mineral acid like hydrochloric acid or alkali like sodium hydroxide solution for a few minutes to remove any layer of oxidation that prevents it from reacting, after this rinse with distilled water twice and use immediately else store under non-polar liquid until ready use required.
However in this reduction of nitroalkene to ketone, hydrochloric acid is one of the reagents, therefore activation can occur in situ.
75ml of distilled water
0.1g of ferric chloride - acts as an initialization catalyst - helps reaction start faster
Acid from addition funnel is added slowly over 5 to 6 hours, so as to keep the reaction going but not explosively so, reflux should never reach over half way up the reflux condenser.
At the end the reaction mixture was then basified with 25% NaOH solution until pH 11 and then steam distill the P2P oil over to a receiver.
Yield should be 75 to 77% P2P from the P2NP ie. P2P 134.3 g/mol so 0.1 mole is 13.42g and 0.75 to 0.77 % yield = 10g (9.94ml) to 10.3g (10.24ml) (Density of P2P is 1.006 g/mL)
This reaction can be scalled up to quite a large size, the molar equivalents are:
molar ratio of Fe/alkene = 7.15
molar ratio of HCl/Alkene = 1.97
1.97 x 0.1 mole of p2NP=0.197 moles of HCl x HCl 36.458 g/mol = 7.18g HCl
if you have concentrated hydrochloric acid 35.5% that means it has 355g/L, or 35.5g/100ml so 718g / 0.355 = 20.2ml of concentrated hydrochloric acid 35.5% to be added via addition funnel
So a 1 mole reaction would use a 5L RBF with 163.2 g of P2NP, 7.15 mole of Fe (7.15 x 55.85 g/mol) = 400g of iron powder, 750ml of distilled water, 1g of Ferric Chloride and 202ml of concentrated hydrochloric acid 35.5%
Yield would be 100g (99.4ml) to 103g (102.4ml) of P2P
Note: For a cheap overhead stirrer:
From ebay you can get a cheap PTFE stirrer bearing to fit the correct size of your boiling flask central neck, you can get a steel stirrer coated in PTFE to protect it from the acid, you can get a bench supply that supplies 0-30V 0-3A for about £30, and you can get a DC motor from certain handheld blenders cheap which you can take apart and connect motor shaft to stirrer shaft, stirrer shaft goes through bearing (pre-grease internal bearing ring with vaseline to help reduce friction), connect the motor to the bench power supply, set the current high enough to supply to motor, then vary speed by increasing/decreasing voltage.
PTFE Standard Stopper Lab Stirrer Bearing Adapter Stirrer Accessory No.29
https://www.ebay.co.uk/itm/313672059695
£10.84
This will fit a 29/32 socket on a boiling flask, it uses a stirrer shaft of 8mm diameter
Findind a PTFE coated stirrer with shaft diameter 8mm tricky most on ebay 7mm so it maybe best to order both items from laborxing that's 2 weeks to arrive but they have high quality equipment.
https://www.laborxing.com/products/ptfe-stirrer-bearing-adapter-joint-stopper
https://www.laborxing.com/products/ptfe-stirring-blades-propeller-2-winged-length-250-mm-to-750-mm
Bench power supply 0-30V 0-10A - potentially this is powerful enough to run electrochemical reactions, and peltier cooling modules
https://www.amazon.co.uk/dp/B09ZQBFZ4C
£44.99
You should be able to find a cheaper one because you only need 0-3A, maybe if the motor you pick up is high torque then 0-5A
Add to a 500ml Round bottomed boiling flask (RBF) with 3 necks
central neck has an overhead stirrer - IMPORTANT has to be an overhead stirrer and has to be powerful enough to keep iron powder from settling on the bottom, cannot use magnetic stirring as it does not have enough power to keep the iron powder up in the solution and the iron messes with the magnetic stirring anyway.
side neck has a long reflux condenser with cold water supplied
2nd side neck has a pressure-equalising addition funnel filled with 0.197 mole of conc. hydrochloric acid 35.5% in the below example thats is 20.2 ml
The RBF is in a water or oil bath to keep internal reaction temperature at 85 to 95 degC.
Add to RBF:
0.1 mole of P2NP (P2NP 163.2 g/mole) = 16.23g of P2NP
0.715 mole of iron (Fe 55.85 g/mole) = 40g of iron (Fe) - cast iron turnings or ideally 40 mesh iron powder (powder 0.4 mm size)
Note: Activate a metal normally involves rinsing it with a strong mineral acid like hydrochloric acid or alkali like sodium hydroxide solution for a few minutes to remove any layer of oxidation that prevents it from reacting, after this rinse with distilled water twice and use immediately else store under non-polar liquid until ready use required.
However in this reduction of nitroalkene to ketone, hydrochloric acid is one of the reagents, therefore activation can occur in situ.
75ml of distilled water
0.1g of ferric chloride - acts as an initialization catalyst - helps reaction start faster
Acid from addition funnel is added slowly over 5 to 6 hours, so as to keep the reaction going but not explosively so, reflux should never reach over half way up the reflux condenser.
At the end the reaction mixture was then basified with 25% NaOH solution until pH 11 and then steam distill the P2P oil over to a receiver.
Yield should be 75 to 77% P2P from the P2NP ie. P2P 134.3 g/mol so 0.1 mole is 13.42g and 0.75 to 0.77 % yield = 10g (9.94ml) to 10.3g (10.24ml) (Density of P2P is 1.006 g/mL)
This reaction can be scalled up to quite a large size, the molar equivalents are:
molar ratio of Fe/alkene = 7.15
molar ratio of HCl/Alkene = 1.97
1.97 x 0.1 mole of p2NP=0.197 moles of HCl x HCl 36.458 g/mol = 7.18g HCl
if you have concentrated hydrochloric acid 35.5% that means it has 355g/L, or 35.5g/100ml so 718g / 0.355 = 20.2ml of concentrated hydrochloric acid 35.5% to be added via addition funnel
So a 1 mole reaction would use a 5L RBF with 163.2 g of P2NP, 7.15 mole of Fe (7.15 x 55.85 g/mol) = 400g of iron powder, 750ml of distilled water, 1g of Ferric Chloride and 202ml of concentrated hydrochloric acid 35.5%
Yield would be 100g (99.4ml) to 103g (102.4ml) of P2P
Note: For a cheap overhead stirrer:
From ebay you can get a cheap PTFE stirrer bearing to fit the correct size of your boiling flask central neck, you can get a steel stirrer coated in PTFE to protect it from the acid, you can get a bench supply that supplies 0-30V 0-3A for about £30, and you can get a DC motor from certain handheld blenders cheap which you can take apart and connect motor shaft to stirrer shaft, stirrer shaft goes through bearing (pre-grease internal bearing ring with vaseline to help reduce friction), connect the motor to the bench power supply, set the current high enough to supply to motor, then vary speed by increasing/decreasing voltage.
PTFE Standard Stopper Lab Stirrer Bearing Adapter Stirrer Accessory No.29
https://www.ebay.co.uk/itm/313672059695
£10.84
This will fit a 29/32 socket on a boiling flask, it uses a stirrer shaft of 8mm diameter
Findind a PTFE coated stirrer with shaft diameter 8mm tricky most on ebay 7mm so it maybe best to order both items from laborxing that's 2 weeks to arrive but they have high quality equipment.
https://www.laborxing.com/products/ptfe-stirrer-bearing-adapter-joint-stopper
https://www.laborxing.com/products/ptfe-stirring-blades-propeller-2-winged-length-250-mm-to-750-mm
Bench power supply 0-30V 0-10A - potentially this is powerful enough to run electrochemical reactions, and peltier cooling modules
https://www.amazon.co.uk/dp/B09ZQBFZ4C
£44.99
You should be able to find a cheaper one because you only need 0-3A, maybe if the motor you pick up is high torque then 0-5A
P2np to p2p
Add to a 500ml Round bottomed boiling flask (RBF) with 3 necks
central neck has an overhead stirrer - IMPORTANT has to be an overhead stirrer and has to be powerful enough to keep iron powder from settling on the bottom, cannot use magnetic stirring as it does not have enough power to keep the iron powder up in the solution and the iron messes with the magnetic stirring anyway.
side neck has a long reflux condenser with cold water supplied
2nd side neck has a pressure-equalising addition funnel filled with 0.197 mole of conc. hydrochloric acid 35.5% in the below example thats is 20.2 ml
The RBF is in a water or oil bath to keep internal reaction temperature at 85 to 95 degC.
Add to RBF:
0.1 mole of P2NP (P2NP 163.2 g/mole) = 16.23g of P2NP
0.715 mole of iron (Fe 55.85 g/mole) = 40g of iron (Fe) - cast iron turnings or ideally 40 mesh iron powder (powder 0.4 mm size)
Note: Activate a metal normally involves rinsing it with a strong mineral acid like hydrochloric acid or alkali like sodium hydroxide solution for a few minutes to remove any layer of oxidation that prevents it from reacting, after this rinse with distilled water twice and use immediately else store under non-polar liquid until ready use required.
However in this reduction of nitroalkene to ketone, hydrochloric acid is one of the reagents, therefore activation can occur in situ.
75ml of distilled water
0.1g of ferric chloride - acts as an initialization catalyst - helps reaction start faster
Acid from addition funnel is added slowly over 5 to 6 hours, so as to keep the reaction going but not explosively so, reflux should never reach over half way up the reflux condenser.
At the end the reaction mixture was then basified with 25% NaOH solution until pH 11 and then steam distill the P2P oil over to a receiver.
Yield should be 75 to 77% P2P from the P2NP ie. P2P 134.3 g/mol so 0.1 mole is 13.42g and 0.75 to 0.77 % yield = 10g (9.94ml) to 10.3g (10.24ml) (Density of P2P is 1.006 g/mL)
This reaction can be scalled up to quite a large size, the molar equivalents are:
molar ratio of Fe/alkene = 7.15
molar ratio of HCl/Alkene = 1.97
1.97 x 0.1 mole of p2NP=0.197 moles of HCl x HCl 36.458 g/mol = 7.18g HCl
if you have concentrated hydrochloric acid 35.5% that means it has 355g/L, or 35.5g/100ml so 718g / 0.355 = 20.2ml of concentrated hydrochloric acid 35.5% to be added via addition funnel
So a 1 mole reaction would use a 5L RBF with 163.2 g of P2NP, 7.15 mole of Fe (7.15 x 55.85 g/mol) = 400g of iron powder, 750ml of distilled water, 1g of Ferric Chloride and 202ml of concentrated hydrochloric acid 35.5%
Yield would be 100g (99.4ml) to 103g (102.4ml) of P2P
Note: For a cheap overhead stirrer:
From ebay you can get a cheap PTFE stirrer bearing to fit the correct size of your boiling flask central neck, you can get a steel stirrer coated in PTFE to protect it from the acid, you can get a bench supply that supplies 0-30V 0-3A for about £30, and you can get a DC motor from certain handheld blenders cheap which you can take apart and connect motor shaft to stirrer shaft, stirrer shaft goes through bearing (pre-grease internal bearing ring with vaseline to help reduce friction), connect the motor to the bench power supply, set the current high enough to supply to motor, then vary speed by increasing/decreasing voltage.
PTFE Standard Stopper Lab Stirrer Bearing Adapter Stirrer Accessory No.29
https://www.ebay.co.uk/itm/313672059695
£10.84
This will fit a 29/32 socket on a boiling flask, it uses a stirrer shaft of 8mm diameter
Findind a PTFE coated stirrer with shaft diameter 8mm tricky most on ebay 7mm so it maybe best to order both items from laborxing that's 2 weeks to arrive but they have high quality equipment.
https://www.laborxing.com/products/ptfe-stirrer-bearing-adapter-joint-stopper
https://www.laborxing.com/products/ptfe-stirring-blades-propeller-2-winged-length-250-mm-to-750-mm
Bench power supply 0-30V 0-10A - potentially this is powerful enough to run electrochemical reactions, and peltier cooling modules
https://www.amazon.co.uk/dp/B09ZQBFZ4C
£44.99
You should be able to find a cheaper one because you only need 0-3A, maybe if the motor you pick up is high torque then 0-5A
Any help is appreciated.