Having a problem here. Let me first start by saying SWFA’s not a numbskull. SWFA can’t believe this failed, SWFA dosent know why this happened. Chromic’s write up was followed to a T with 3 exceptions.
1: The reaction was scaled up x4.
2: A small amount (29.2 grams) of extra oxone was added to the mix because SWFA called the manufacturer of the product and requested a MSDS for the product in question. They told him that they didn’t have the MSDS information available at the time but did say that their product was Ph neutral.
3: All contents were added to an Erlenmeyer flask as opposed to a round bottom flask for stirring reasons.
What SWFA did
2 liters of DH20 were added to the reaction flask.
65 grams of isosafrole were added to the reaction flask
800 ml Methanol were added to the reaction flask
320 grams of oxone were added ( as opposed to the suggested 290.
Added a large 3 inch stir bar
Put a condenser on the flask clod water running just in case
Then cranked the stirrer on full blast (creating a deep vortex in the flask). Aqueous phase temperature was 31.6c. SWFA left this stirring heavily for 5 hours. When SWFA returned and turned the stirrer off the aqueous phase was totally clear no signs of any yellow tint at all. SWFA immediately noticed a problem and decided to stir a little longer. No signs of anything remotely yellow in the flask at the 8-hour mark. It appears the oxone had totally crashed out of solution from the start. The flask looks like a giant snow globe there’s a lot of oxone sitting on the bottom of the reaction flask. When SWFA swirls the flask it’s contents it gives off a few small bubbles.
What is the problem here?
Why is SWFA not seeing the characteristic color changes?
The person who answered SWFA's call at the company didn’t appear to familiar of the product other than the fact that his company puts Dupont oxone in their shocking agent. He said the oxone was Ph neutral but did he really mean ph neutral for 10,000 gallons of water? Did he misinform SWFA? Is the oxone pure?
If the oxone was pure and SWFA didn’t add the buffer would the oxone not liberate enough oxygen to epoxidize his
2-Alkene. Is this the problem?
Any help in this matter would be most appreciated.
EDIT It says on the package that the shocking agen will not affect ph levels. Did SWFA get a bad product blend? Is there a flaw in my method above?
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