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hello
9. Sodium bicarbonate 5% H2O solution 300 ml was poured into flask with freebase then stirred for 30 mins. After that layers are
how much Sodium bicarbonate do you put in the recipe?
9. Sodium bicarbonate 5% H2O solution 300 ml was poured into flask with freebase then stirred for 30 mins. After that layers are
how much Sodium bicarbonate do you put in the recipe?
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- By ghostimage
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15 Apr
you must not use soda on any step of 4mmc, it is produce more problems than solutions, all you need is wash wash wash.
bromination ccan be done with 100% yields with clean result, amination...yes, only 3-5x waterwash, acidation, again, can be done clean way, but at least one wash is must.
bromination ccan be done with 100% yields with clean result, amination...yes, only 3-5x waterwash, acidation, again, can be done clean way, but at least one wash is must.
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Most often purity of 4 methylopropiophenone is 95%, we should know the exact data but if we cant, we use 95%, so for 1 mole of 4 methylopropiophenone we do use one mole of hbr.
4′-methylpropiophenone (CAS 5337-93-9) 1000 g
. Hydrobromic acid 48% aq . 1155 g or 775 ml. Hydrogen peroxide
(H2O2) 35% 980g, (plus 20-30% excess.
H2O2 will decompose during the reaction)
Sodium bicarbonate (NaHCO3) 595.5g,
Distilled water.
Glacial acetic acid 432ml
1. 1000g of 4'-methylprophiophenone is added to the flask.
2. Hydrobromic acid (HBr) 1155 g or 775 ml 48% is poured into the flask and stirred for 5 min. Temperature set to 60c using a water bath.
3. Hydrogen peroxide 35% 1200g is added to the drip funnel.
4. Glacial acetic acid is added through the cooler, wait until it stops "dripping".
5. H2O2 is added in small amounts. Orange/red bromine is released. When the reaction slows down we add acetic acid in small amount, equal to the total amount to be used of h2o2
6. Repeat the steps until you add 50% h2o2.
7. The temperature of the reaction mixture must be increased to 70-75c, after increasing the temperature, the addition of h2o2 and acetic acid can continue.
9. After adding all the reagents, stir at 70-75c for an hour. 10. As a result of lowering the temperature, 2b4m is formed.
Glacial acetic acid is neutralised with equal amount of nahco3 in water.
For futher reaction 90% of purity is starting data.
4′-methylpropiophenone (CAS 5337-93-9) 1000 g
. Hydrobromic acid 48% aq . 1155 g or 775 ml. Hydrogen peroxide
(H2O2) 35% 980g, (plus 20-30% excess.
H2O2 will decompose during the reaction)
Sodium bicarbonate (NaHCO3) 595.5g,
Distilled water.
Glacial acetic acid 432ml
1. 1000g of 4'-methylprophiophenone is added to the flask.
2. Hydrobromic acid (HBr) 1155 g or 775 ml 48% is poured into the flask and stirred for 5 min. Temperature set to 60c using a water bath.
3. Hydrogen peroxide 35% 1200g is added to the drip funnel.
4. Glacial acetic acid is added through the cooler, wait until it stops "dripping".
5. H2O2 is added in small amounts. Orange/red bromine is released. When the reaction slows down we add acetic acid in small amount, equal to the total amount to be used of h2o2
6. Repeat the steps until you add 50% h2o2.
7. The temperature of the reaction mixture must be increased to 70-75c, after increasing the temperature, the addition of h2o2 and acetic acid can continue.
9. After adding all the reagents, stir at 70-75c for an hour. 10. As a result of lowering the temperature, 2b4m is formed.
Glacial acetic acid is neutralised with equal amount of nahco3 in water.
For futher reaction 90% of purity is starting data.