i've come around this novel way and tried to do it , but run into problems i hope you can help me figure it out.
i've ordered 1kg of 2,5 Dmba from china.
this is the steps :
1. Dissolve 8.3g (50mmol) 2,5-Dimethoxy Benzaldehyde in 50ml Methanol and 6.1g(100mmol) Nitromethane in 1L beaker. Stir the solution and cool it to 0~5 degree C.
2. Dissolve 8.4g(150mol) Potassium Hydroxide in 25ml Methanol. Stir the solution and cool it to 0~5 degree C.
3. Place the beaker with 2,5-Dimethoxy Benzaldehyde solution in(1) in a big container with ice-salt baths and setup the big container on the magnetic stirrer. Use thermometer to monitor the temperature inside beaker and turn on stirrer.
4. Use dropper to add Potassium Hydroxide solution slowly into the beaker. Avoid the temperature exceed 5 degree C.
5. After addition is done (typically within 1 hour), stir the mixture for another 30 min.
6. Prepare 300ml 10% HCl solution and cool it to 5-10 degree C when you stir the mixture.
7. Add cooled 10% HCl solution into beaker with mixture in 5 times every 5 min (roughly 60 ml once) with stirring.
8. Now you can see yellow colored crystal inside the mixture. Prepare Buchner funnel and flask and use the suction source to collect the crystal. You do not need to dry and weight the crystal.
***first pic when you see yellow (the darker one is unreacted DMBA ans was removed.
9. Mix 300ml 32% HCl solution and 150ml IPA in 1L beaker. Cool the solution to 5 degree C.
10. Add the wet crystal from (8) into the HCl/IPA solution from (9). Place the beaker in a big container with ice-salt baths and setup the big container on the magnetic stirrer.
11. Prepare 45g zinc powder. Add the powder into the stirring solution within 1 hour. Do not be hurry or you will get many yellow bubble. Use small spoon and add slowly.
12. After addition is done. Stir the mixture for another 2 hour, now you can see the solution become transparent and there might be some un-dissolved zinc in the bottom. On the surface of the un-dissolved zinc powder, you will see very small hydrogen bubble. Put the mixture with cover into the refrigerator for one night. At the same time, mix 100g Sodium Hydroxide with 150ml water. Add NaOH into water in 3 or 4 times to avoid temperature increasing. Put the NaOH solution into the refrigerator, too.
13. Place the beaker with mixture in a big container with ice-salt baths and setup the big container on the magnetic stirrer. Add NaOH solution into the stirring mixture slowly to avoid temperature increasing.
14. After addition is done, another 50g NaCl is added into the mixture and sit the mixture for few hour until you can see the IPA layer well separated.
15. Use dropper to suck the IPA layer carefully into a container. Add 50ml IPA into the mixture and suck to collect the product two times.
16. Put the IPA with 2C-H under a fan to evaporate it. Few hours later, you will get yellow color oil(2C-H). You can mix 200g Sodium Hydroxide with 300ml water. Add NaOH into water in 3 or 4 times to avoid temperature increasing. Put the NaOH solution into the refrigerator.
17. Weight the oil and record it. If you have scale upper limit issue, prepare a smaller container and record the empty weight. During IPA evaporation, you can transfer the mixture into the smaller container.
*** PIC here i got the 2ch extracted with dmba with ipa and was dried (my 2ch was kinda dark looking even tho i really watched temperature.
18. For 100mmol 2C-H, dissolve it in 50ml GAA in a 1L beaker and put the beaker into ice bath on stirrer.
19. Mix 120ml GAA, 40ml water, 11.8g Sulfuric acid(120mmol) and 14.3g Potassium Bromide(120mmol) into another beaker. Add 5.8g 35% hydrogen peroxide solution(60mmol) into the mixture with stirring. You will see the color changed.
20. Use dropper to add the mixture from (19) into the mixture from (18) slowly with stirring. After addition is done, add 5.8g 35% hydrogen peroxide solution(60mmol) into the mixture with stirring. Wait for another 20 min with stirring.
*here is the brommination stage , i think i got it right ... just mix all the things together.
21. Add NaOH solution from (16) into the mixture in ice-bath slowly.
* thats the picture with the black goo floating
22. The color should be dark brown now. Add 100ml Toluene into the mixture with stirring. After 5 min stirring, sit the mixture to wait the layer separation. Suck the Toluene out by dropper and collect the Toluene. Repeat this step until the Toluene become transparent. You need to add Toluene maybe 3 times or more depends on your skill.
*add the pic with soluene extraction with the layers . i then also used a separatory funnel to make sure the toluene was as clean as possible with no water in it.
23. Put the Toluene on stirrer and add 13.6g 32% HCl solution(120mmol). With stirring, you will see some salt generated in the Toluene. Few minutes later, stop stirring and use funnel and filter to collect the salt powder. It should be dark brown color.
***thats where i can into a problem , i add hcl to the toluene , and instead of salt generated , just a black goo is generated that drops to the bottom and i endded up with a large amount of it T_T
24. Use Acetone to wash the powder on filter by dropper until the color become white.
now i really dont know what to do? , i have that black goo that sinked at the bottom , i guess is 2cb ? that cant form salt? and it became protenated and became insolubale at toluene and sinked at the bottom ?
i have access to DCM i wonder what should i do next? should i collect the black sinked goo and do something with it ?
also my 2ch oil was kinda dark looking , is this significant ?
i've ordered 1kg of 2,5 Dmba from china.
this is the steps :
1. Dissolve 8.3g (50mmol) 2,5-Dimethoxy Benzaldehyde in 50ml Methanol and 6.1g(100mmol) Nitromethane in 1L beaker. Stir the solution and cool it to 0~5 degree C.
2. Dissolve 8.4g(150mol) Potassium Hydroxide in 25ml Methanol. Stir the solution and cool it to 0~5 degree C.
3. Place the beaker with 2,5-Dimethoxy Benzaldehyde solution in(1) in a big container with ice-salt baths and setup the big container on the magnetic stirrer. Use thermometer to monitor the temperature inside beaker and turn on stirrer.
4. Use dropper to add Potassium Hydroxide solution slowly into the beaker. Avoid the temperature exceed 5 degree C.
5. After addition is done (typically within 1 hour), stir the mixture for another 30 min.
6. Prepare 300ml 10% HCl solution and cool it to 5-10 degree C when you stir the mixture.
7. Add cooled 10% HCl solution into beaker with mixture in 5 times every 5 min (roughly 60 ml once) with stirring.
8. Now you can see yellow colored crystal inside the mixture. Prepare Buchner funnel and flask and use the suction source to collect the crystal. You do not need to dry and weight the crystal.
***first pic when you see yellow (the darker one is unreacted DMBA ans was removed.
9. Mix 300ml 32% HCl solution and 150ml IPA in 1L beaker. Cool the solution to 5 degree C.
10. Add the wet crystal from (8) into the HCl/IPA solution from (9). Place the beaker in a big container with ice-salt baths and setup the big container on the magnetic stirrer.
11. Prepare 45g zinc powder. Add the powder into the stirring solution within 1 hour. Do not be hurry or you will get many yellow bubble. Use small spoon and add slowly.
12. After addition is done. Stir the mixture for another 2 hour, now you can see the solution become transparent and there might be some un-dissolved zinc in the bottom. On the surface of the un-dissolved zinc powder, you will see very small hydrogen bubble. Put the mixture with cover into the refrigerator for one night. At the same time, mix 100g Sodium Hydroxide with 150ml water. Add NaOH into water in 3 or 4 times to avoid temperature increasing. Put the NaOH solution into the refrigerator, too.
13. Place the beaker with mixture in a big container with ice-salt baths and setup the big container on the magnetic stirrer. Add NaOH solution into the stirring mixture slowly to avoid temperature increasing.
14. After addition is done, another 50g NaCl is added into the mixture and sit the mixture for few hour until you can see the IPA layer well separated.
15. Use dropper to suck the IPA layer carefully into a container. Add 50ml IPA into the mixture and suck to collect the product two times.
16. Put the IPA with 2C-H under a fan to evaporate it. Few hours later, you will get yellow color oil(2C-H). You can mix 200g Sodium Hydroxide with 300ml water. Add NaOH into water in 3 or 4 times to avoid temperature increasing. Put the NaOH solution into the refrigerator.
17. Weight the oil and record it. If you have scale upper limit issue, prepare a smaller container and record the empty weight. During IPA evaporation, you can transfer the mixture into the smaller container.
*** PIC here i got the 2ch extracted with dmba with ipa and was dried (my 2ch was kinda dark looking even tho i really watched temperature.
18. For 100mmol 2C-H, dissolve it in 50ml GAA in a 1L beaker and put the beaker into ice bath on stirrer.
19. Mix 120ml GAA, 40ml water, 11.8g Sulfuric acid(120mmol) and 14.3g Potassium Bromide(120mmol) into another beaker. Add 5.8g 35% hydrogen peroxide solution(60mmol) into the mixture with stirring. You will see the color changed.
20. Use dropper to add the mixture from (19) into the mixture from (18) slowly with stirring. After addition is done, add 5.8g 35% hydrogen peroxide solution(60mmol) into the mixture with stirring. Wait for another 20 min with stirring.
*here is the brommination stage , i think i got it right ... just mix all the things together.
21. Add NaOH solution from (16) into the mixture in ice-bath slowly.
* thats the picture with the black goo floating
22. The color should be dark brown now. Add 100ml Toluene into the mixture with stirring. After 5 min stirring, sit the mixture to wait the layer separation. Suck the Toluene out by dropper and collect the Toluene. Repeat this step until the Toluene become transparent. You need to add Toluene maybe 3 times or more depends on your skill.
*add the pic with soluene extraction with the layers . i then also used a separatory funnel to make sure the toluene was as clean as possible with no water in it.
23. Put the Toluene on stirrer and add 13.6g 32% HCl solution(120mmol). With stirring, you will see some salt generated in the Toluene. Few minutes later, stop stirring and use funnel and filter to collect the salt powder. It should be dark brown color.
***thats where i can into a problem , i add hcl to the toluene , and instead of salt generated , just a black goo is generated that drops to the bottom and i endded up with a large amount of it T_T
24. Use Acetone to wash the powder on filter by dropper until the color become white.
now i really dont know what to do? , i have that black goo that sinked at the bottom , i guess is 2cb ? that cant form salt? and it became protenated and became insolubale at toluene and sinked at the bottom ?
i have access to DCM i wonder what should i do next? should i collect the black sinked goo and do something with it ?
also my 2ch oil was kinda dark looking , is this significant ?
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