ahgreich (Hive Bee)
03-03-04 16:59
No 492823
      possible solvent-supported Hypo method?     

prep:
1. dissolve pseudo fb in ether, beaker #1.
2. extract hypophosphorus acid from the aqueous with ether, separate ethereal solution into beaker #2.
3. dissolve iodine in ether, beaker # 3.

reaction:
a. combine solutions from beaker # 1 and #2.
b. slowly drip iodine ethereal solution from beaker #3 into solution 'a'.
either gently reflux solution 'b', or allow to sit for some time at room temperature (what do bees think?).

workup:
reclaim iodine and hypo (as sodium hypophosphite) by washing ethereal solution with dh20 basified with NaOH, thereby leaving the meth fb in the ether.
wash the ether with dh20 several times.
gas, titrate, or whatever the ether for meth hcl.

would the hypo and I form HI, and would it stay in ethereal solution, escape as a gas, or react with the ether to create something weird?
if it formed HI and stayed in solution, would the rxn take place at room temp?
 
 
 
 
    SpicyBrown
(Hive Bee)
03-03-04 23:21
No 492892
      Ether probably wouldn't be ideal, as HI is...     

Ether probably wouldn't be ideal, as HI is frequently used to cleave ethers.

-SpicyBrown