bones (Stranger)
05-06-03 13:05
No 431704
      1,2 methylenedioxybenzene synth solvent switch?  Bookmark   

hey...my lab sucks... all these chemicals but no methylenedioxybenzene... but i think i can make some from catachol ... theres a synth on rhodiums page and ive been checking out scifinder... BUT ... we dont have much dmso lying around... so i was hoping to discuss which solvents would be suitable? ... perhaps THF?

heres the prep which appears on rhodiums page... thankx guys

A solution of 110 g of catechol, 120 ml of 50% aqueous sodium hydroxide and 200 ml of DMSO was heated to 98°C and stirred at that temperature for 30 minutes. This solution at 98°C. was added over a 30 minute period to a refluxing solution of 120 ml of methylene dichloride in 300 ml of DMSO. Thereafter, the reaction mixture was stirred at reflux for 1.5 hours. Steam was then passed into the mixture to achieve steam distillation of the product. The distillate (600 ml) was extracted with 100 ml of methylene dichloride, which extract was washed once with 50 ml of water. The methylene dichloride solution was then concentrated in vacuo at 40°C. to yield 119.4 g. of a colorless oil. Gas chromatographic analysis showed 97.5 percent methylenedioxybenzene. Yield 116.4g (95.4%).
 
 
 
 
    murmur
(HyperLab Bee)
05-06-03 13:20
No 431710
      Solvent  Bookmark   

If you wanna get high yield, use DMSO. Others methods I know give yield about 50-60%
 
 
 
 
    Aurelius
(Hive Addict)
05-06-03 19:32
No 431753
      DMF  Bookmark   

Post 398771 (Aurelius: "Preparation of Methylenedioxybenzene (as is TSII?)", General Discourse)
Use Example 5, it doesn't use DMSO.  Yield about 54%. 

BTW, DMSO is OTC.  (at least in US)
 
 
 
 
    Rhodium
(Chief Bee)
05-07-03 02:31
No 431803
      1,2 methylenedioxybenzene  Bookmark   

This doesn't use DMSO either: ../rhodium/chemistry /safrole.html
 
 
 
 
    bones
05-07-03 03:12
      dmso may or may not be otc whre i am...
(Rated as: insignificant)
 Bookmark   
 
 
 
    fallen_Angel
(Гиперконструктор)
05-07-03 06:33
No 431854
      methylenedioxybenzene  Bookmark   

See in Russian:Post 429296 (fallen_Angel: "Бензодиоксол", Russian HyperLab)

I did by miscellaneous expedients, best through DMSO, yield 70-80 %. All other are worse and on a yield, and is more  worse to do.