Well, it may not be a breakthrough, but swim's a fan of alliteration. Anyways . . .
A funny thing happened to swim not long ago in a vivid dream. Swim was making benzoquinone using the h2o2/i2 method (3x scale) as posted on rhodium's site. Swim placed the hydroquinone/iodine/ipa in a water bath of 30c and waited for all the hydro to dissolve. Swim then set a drip rate of h2/02 of about 1.5 drips per second. This may sound fast, but in the past when luke warm water baths were used, the addition of h202 produced only a minor temp change through until the end of addition. Swim then went out to the store for more ipa and ice and what not and came back to find his reaction mixture thouroughly boiling. Swim immediately pulled the flask out of the water bath (which was only 32c) and swirled the contents to find that absolutely everything has dissolved into the solution after a few swirls. The flask was immediately placed in an ice bath and immediate crystallization of benzo occured. The mixture was cooled to 10c and the liquid was decanted off of the benzo crystals. Recrystallized in 91% ipa and did a final wash with ice cold ipa to yield 145.1g of absolutely beautiful yellow benzo shards. W/W yield (molecular almost the same) comes out to be 88%. only 3 percentage points less than the yield claimed on the patent.
Why is this significant? The reaction took place in under half an hour. Let swim repeat that. One half hour. That's enough benzo for a full scale wacker at next to no cost, effort, or time.
Swim decided to repeat this accident. The following dream took place just tonight in the back of Swim's sleepy head.
345g 91% ipa and 1.5g I2 (this is half the amount specified by the patent at this scale, but swim believe this is still more than necessary) were stirred in a 1000ml erlenmeyer flask until complete dissolution of the i2 crystals occured. 165g of hydroquinone was added to the solution and the flask was placed in a luke warm water bath of and set atop a magnetic stirrer. When all the hydro was stirred into the solution, 185g 30% h2/o2 was added at a rate of just over one drop per second. All of the h2o2 was added with little temperature evolution noted. When the addition was complete, the water bath was heated until the reaction mixture started to boil. This was allowed to proceed for about 2 minutes and the flask was then removed from the water bath. Quinhydrone was seen collected at edges of the bottom of the flask. Swirling the mixture caused complete dissolution of all solids present. This was allowed to sit for 5 minutes (swim thought that the quinhydrone he just swirled into the solution might need a little time to react. After 5 minutes, the flask was plunged into an ice bath and the temperature of the solution was brough to 10c. The liquid was decanted off and the remaining benzo was recrystallized with 160 ml of 91% ipa and washed a final time with freezing cold ipa to yield 144 of some of the most gorgeous benzo swim's made yet. 87% yield, 1/16 reaction time.....yeah, swim's hooked.
Swim used to perform this reaction by adding h2o2 at a rate such as to keep the temp at 35c, then after the addition apply external heat to bring the solution to 45c, as per the patent. At 3x or greater scale, swim never had a benzo reaction complete in less than 8 hours at these temps. The reaction above took less than half an hour. That equates to a reduction of reaction time by 93.8%, AND half as much iodine was used at called for in the patent, AND no temperature monitoring was needed.
Swim's going to try it again tonight, but this time 33% less iodine will be used and the reaction mixture will be plunged into an ice bath immediately after the three minutes of boiling. Also, for those of you that wish to try this method, be forewarned that not using a contained system with reflux will result in the room smelling of ipa and benzo. Swim found this can be contained pretty well by using a square of al foil over the top of the flask.
Will report later on next dream.
p.s. This is swim's first post and swim would like to thank everyone at the hive for their collective knowledge. Rock on.